CN103232236A - A method for preparing high dielectric tuning ceramic (Ba, sr) TiO3with excessive TiO2 - Google Patents

A method for preparing high dielectric tuning ceramic (Ba, sr) TiO3with excessive TiO2 Download PDF

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CN103232236A
CN103232236A CN2013101412803A CN201310141280A CN103232236A CN 103232236 A CN103232236 A CN 103232236A CN 2013101412803 A CN2013101412803 A CN 2013101412803A CN 201310141280 A CN201310141280 A CN 201310141280A CN 103232236 A CN103232236 A CN 103232236A
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金灯仁
周立新
谢朝军
董汉莛
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a preparation method of (Ba,Sr)TiO3 (BST) ceramic having high tunability and high temperature stability, belonging to the technical field of preparation of special ceramics for a wireless communication technology. The BST ceramic is prepared by taking BaCO3, TiO2 and SrCO3 as raw materials, combining a solid-phase reaction method, an ice bath ultrasonic method and a sol-permeable auxiliary sintering technology, adding TiO2 into a BaTiO3/SrTiO3 mixed-phase biscuit and sintering at a low sintering temperature (1280 DEG C); and the tunability of the BST ceramic is 36.9% (room temperature/10KHz), the dielectric loss is less than 0.03 (room temperature/100Hz-10MHz), and the BST ceramic has high temperature stability. The invention provides a feasible method for preparing BST dielectric ceramic having high tunability and high temperature stability, which is simple in process, low in production cost and easy to realize mass production.

Description

A kind of TiO 2Excessive high dielectric tuning pottery (Ba, Sr) TiO 3The preparation method
Technical field
The present invention relates to microwave device dielectric tuning (Ba, Sr) TiO that a kind of preparation has high tuning rate, high-temperature stability 3The new technology of dielectric ceramics belongs to wireless communication technology special cermacis preparing technical field.
Background technology
The specific inductivity of strontium-barium titanate (BST) material can change with extra electric field, be a kind of adjustable main research material of dielectric that can be applicable under the microwave, have potential application prospect in the tunable oscillator in the phase shifter in phased array antenna system/radar and the microwave wireless communication system, the tunable optic filter etc.These use the performance requriements that the BST pottery is proposed: lofty tone harmonic quantity, high-temperature stability, low-loss and suitable dielectric coefficient.Improving dielectric tuning rate, temperature stability and reducing the wastage still is the main task in current BST ceramic research field.
BST is BaTiO 3With SrTiO 3The complete solid solution system that forms.BaTiO 3(BT) and SrTiO 3(ST) all belong to ABO 3Type perovskite structure ferroelectric material, their infinitely solid solutions form single uhligite phase, and transformation temperature is adjustable with the Ba/Sr linearity, can obtain the tuning rate maximum at the transformation temperature place.
Many research work are round the material that how to obtain near the high dielectric tuning rate room temperature, and the preparation Curie temperature is near the BST composite ceramics of room temperature.GuoxinHu etc. have prepared near Curie temperature Ba room temperature 0.6Sr 0.4TiO 3– MgAl 2O 4Pottery, result of study shows 70wt%Ba 0.6Sr 0.4TiO 3– 30wt%MgAl 2O 4It is 23.63%(1KV/mm that pottery is obtained maximum tuning rate), and the specific inductivity temperature stability is relatively poor, the dielectric properties instability influences the works better of device.The Xiaohong Wang of the Central China University of Science and Technology has prepared doping 0.2wt% La through 1550 ℃ of sintering 2O 3Ba 0.6Sr 0.4TiO 3-MgO complex phase ceramic, the room temperature dielectric tuning rate of sample is 16.26% (3.57KV/mm), loss is 0.012(2.853GHz); The Xu Honghai of this study group has prepared Ba 0.75Sr 0.25TiO 3The heterogeneous body pottery, the sample of 1340 ℃ and 1400 ℃ sintering, room temperature dielectric tuning rate is respectively 16.6% and 21.5% (1KV/mm).
The invention provides the BST pottery new preparation technology that a kind of technology is simple, with low cost, be easy to produce in batches and have high dielectric tuning rate, high-temperature stability.
Summary of the invention
The object of the present invention is to provide (Ba, Sr) TiO of a kind of high dielectric tuning rate, high-temperature stability 3The preparation method of pottery.
A kind of TiO of the present invention 2Excessive high dielectric tuning pottery (Ba, Sr) TiO 3The preparation method, it is characterized in that having following preparation process and step:
(A), TiO 2Excessive (Ba, Sr) TiO 3The preparation of mixed phase powder
A. with BaCO 3, SrCO 3And TiO 2Be raw material, adopt solid reaction process, respectively at 1100 ℃, 1200 ℃ synthetic BaTiO 3(being called for short BT), SrTiO 3(being called for short ST) powder;
B. the back of above-mentioned synthetic good BT and ST powder porphyrize being sieved takes by weighing BT and ST powder according to the ratio of mol ratio BT: ST=3:1, with both mixing; Again according to weight ratio TiO 2: (BT+ST)=1～2% take by weighing TiO 2Powder adds in BT and the ST powder mix and fully mixes, and obtains TiO 2Excessive (Ba, Sr) TiO 3The mixed phase powder;
(B), TiO 2Excessive (Ba, Sr) TiO 3The preparation of mixed phase biscuit
A. with above-mentioned TiO 2Excessive (Ba, Sr) TiO 3The mixed phase powder carries out granulation, and is dry-pressing formed, depresses to disk shape sample at static pressure such as 220MPa then;
B. utilize the ice-bath ultrasonic legal system to be equipped with Ba 0.75Sr 0.25TiO 3Colloidal sol; Take by weighing the Ba (OH) of 0.03mol 28H 2The SrAc of O, 0.01mol 2Mix extremely clarification of ultrasonic dissolution under the room temperature of back with 16ml HAc; The benzene that adds the alcohol of positive four butyl esters of metatitanic acid, 12ml of 0.04mol and 5ml in another clean beaker mixes, ultrasonic dissolution is to clarification; Two portions of ultrasonic clear liquors are mixed, carry out ice-bath ultrasonic, reach clear, get Ba 0.75Sr 0.25TiO 3Colloidal sol;
C. disk shape sample is put into the above-mentioned Ba for preparing 0.75Sr 0.25TiO 3Vacuumize in the colloidal sol and ooze
The saturating processing, 700 ℃ of pre-burnings make TiO then 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit;
(C), the preparation of high-performance BST pottery
With above-mentioned pre-burned TiO 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit obtains BST pottery fine and close, that have high tuning rate, high-temperature stability at 1250 ℃～1280 ℃ sintering temperatures.
The present invention adopts the mixed phase sintering of traditional solid reaction process, in conjunction with colloidal sol infiltration assisted sintering technology, by at (Ba, Sr) TiO 3Insert excessive TiO in the mixed phase biscuit 2Prepare the BST pottery of high dielectric tuning rate, high-temperature stability.Material preparation process of the present invention is simple, and low cost of manufacture is conducive to realize industrial scale production.
Description of drawings
BST pottery preparation flow figure described in Fig. 1 the present invention;
X-ray diffraction (XRD) figure of the BST pottery described in Fig. 2 the present invention;
Profile scanning electron microscope (SEM) the photo figure of the BST pottery described in Fig. 3 the present invention;
The dielectric properties figure of the BST pottery described in Fig. 4 the present invention;
The dielectric tuning figure of the BST pottery described in Fig. 5 the present invention.
Embodiment
Embodiment
Preparation process and step in the present embodiment are as follows:
(A), TiO 2Excessive (Ba, Sr) TiO 3The preparation of mixed phase powder
A. with BaCO 3, SrCO 3(Fen Xi Chun ≧ 99%) and TiO 2(Hua Chun ≧ 98%) is raw material, takes by weighing BaCO respectively according to the stoichiometric ratio 1:1 of BT and ST 3, TiO 2And SrCO 3, TiO 2Put into ball grinder; The zirconia balls mill that adds proper amount of deionized water, dehydrated alcohol and different diameter sizes and shape, ratio of grinding media to material is 2:1, the shared liquid level of deionized water and dehydrated alcohol is about 2/3 of whole ball milling jar height, and the ball grinder rotating speed is 50 rev/mins, and the ball milling time is 24 hours;
B. take out the good slurry of ball milling and sieve in 120 ℃ of oven dry porphyrizes, obtain even fine powder; Place sintering oven to calcine powder, at two hours synthetic BT powder of 1100 ℃ of calcinings, at two hours synthetic ST powder of 1200 ℃ of calcinings;
C. will synthesize good BT and ST powder porphyrize respectively and sieve, and follow according to mol ratio BT: ST=3: 1 mixes both in beaker; Again according to weight ratio TiO 2: (BT+ST)=1～2% take by weighing TiO 2Raw material powder adds in BT and the ST powder mix;
D. with above-mentioned powder mix (BT+ST+TiO 2) ball grinder of packing into carried out ball milling 24 hours, poured out the good slurry of ball milling, dried and sieved, and obtained TiO 2Excessive (Ba, Sr) TiO 3The mixed phase powder;
(B), moulding
A. with the above-mentioned TiO that makes 2Excessive (Ba, Sr) TiO 3It is 7% PVA binding agent that the mixed phase powder adds an amount of concentration, carries out granulation;
B. with above-mentioned TiO after granulation 2Excessive (Ba, Sr) TiO 3The mixed phase powder is dry-pressing formed, depresses to the disk shape sample of diameter 12mm, thickness 1mm then at static pressure such as 220MPa;
C. with sample 700 ℃ of slow binder removals in sintering oven, remove organism such as PVA, obtain TiO 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit;
(C), Ba 0.75Sr 0.25TiO 3The preparation of colloidal sol
A. utilize the ice-bath ultrasonic legal system to be equipped with Ba 0.75Sr 0.25TiO 3Colloidal sol; With Ba (OH) 28H 2O, strontium acetate, glacial acetic acid, Ti (OC 4H 9) 4, dehydrated alcohol, benzene be raw material, takes by weighing the Ba (OH) of 0.03mol 28H 2O is measured 16ml HAc and is poured the beaker mixing in a clean beaker, adds the SrAc of 0.01mol then 2Ultrasonic dissolution is to clarification;
B. the benzene that adds the alcohol of positive four butyl esters of metatitanic acid, 12ml of 0.04mol and 5ml in the clean beaker of another one mixes, ultrasonic dissolution is to clarification;
C. two portions of ultrasonic clear liquors are mixed, carry out ice-bath ultrasonic, reach clear, get the Ba of 0.75mol/L 0.75Sr 0.25TiO 3Colloidal sol;
(D), osmotic treated and pre-burning
A. the TiO that above-mentioned binder removal is crossed 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit is put into the Ba for preparing 0.75Sr 0.25TiO 3Vacuumized osmotic treated in the colloidal sol 30 minutes;
B. will be through Ba 0.75Sr 0.25TiO 3The TiO of colloidal sol osmotic treated 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit is put into 700 ℃ of pre-burnings of sintering oven 2 hours;
(E), sintering
With above-mentioned gained through Ba 0.75Sr 0.25TiO 3The TiO of colloidal sol infiltration and pre-burning 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit obtains fine and close BST ceramics sample 1250 ℃～1280 ℃ sintering temperatures 4 hours.
Whole preparation flow sees that Figure of description is shown in Figure 1, and the ceramics sample of preparation is characterized and does the test of dielectric and tuning performance.
1. X-ray diffractometer (XRD) detects
Detected result is seen Fig. 2, and (a) figure explanation all samples all forms the uhligite phase, does not detect dephasign; (b) the figure explanation improves sintering temperature, and (111) peak FWHM of sample reduces, Ba in BST pottery when low-temperature sintering is described 2+And Sr 2+Mutual diffusion not exclusively, i.e. the formation of compositional gradient in the BST pottery is a kind of heterogeneous body pottery; Than BST, TiO 2Excessive (Ba, Sr) TiO 3The FWHM at (111) peak become big, the adding of titanium dioxide has reduced Ba 2+And Sr 2+The mutual diffusion degree, the component non-uniform degree strengthens.
2. scanning electronic microscope (SEM) detects
Detected result is seen Fig. 3, the employing TiO of Fig. 3 for obtaining among the present invention 2Excessive (Ba, Sr) TiO 3BST pottery and (Ba, Sr) TiO of preparation 3The scanning electron microscope diagram of pottery section.As can be seen from Figure 3, identical sintering schedule (1280 ℃/4h) under, excessive TiO 2Insert, the average grain size that makes sample is varied down to 1.5 microns from 2.5 microns, and grain size range strengthens; Pore quantity is more or less the same, and density is suitable.
3. dielectric properties test
Detected result is seen Fig. 4, the employing TiO that Fig. 4 obtains for 1280 ℃/4h sintering among the present invention 2Excessive (Ba, Sr) TiO 3BST pottery and (Ba, Sr) TiO of preparation 3Dielectric thermogram under pottery room temperature dielectric frequency spectrum and the 100KHz.From (a) figure, find out excessive TiO 2Adding sample room temperature dielectric constant and dielectric loss are all decreased.From (b) figure as can be seen, excessive TiO 2Adding the dielectric loss of sample is obviously reduced, the dielectric peak is significantly downgraded and broadening, temperature stability improves.
4. dielectric tuning rate test
Detected result is seen Fig. 5. the employing TiO that Fig. 5 (a) obtains for 1280 ℃/4h sintering among the present invention 2Excessive (Ba, Sr) TiO 3The preparation the BST pottery at room temperature specific inductivity with the variation relation figure of applying direct current electric field.Utilize formula:
Figure 898449DEST_PATH_IMAGE001
(wherein
Figure 712821DEST_PATH_IMAGE002
With
Figure 662847DEST_PATH_IMAGE003
Being respectively the direct current biasing electric field is zero-sum E AppThe time specific inductivity) tuning rate that calculates is respectively 36.9%(10KHz).
The employing TiO that Fig. 5 (b) obtains for 1280 ℃/4h sintering among the present invention 2Excessive (Ba, Sr) TiO 3BST pottery and (Ba, Sr) TiO of preparation 3Specific inductivity under the ceramic 1KHz at room temperature is with the variation relation figure of applying direct current electric field.1～2wt%TiO as can be seen 2Insert, make (Ba, Sr) TiO 3The tuning rate of pottery significantly brings up to 32.6% from 9.3%.
The result shows, compares with above-mentioned pertinent literature results reported, as (Ba, Sr) TiO of the 1340 ℃/2h sintering such as Xu Honghai of better performances 3Pottery (10KV/cm) compare, and the dielectric tuning rate of the BST pottery of the present invention's preparation is obviously higher, and temperature stability is better by tuning rate 15.2%.

Claims (1)

1. TiO 2Excessive high dielectric tuning pottery (Ba, Sr) TiO 3The preparation method, it is characterized in that having following preparation process and step:
(A), TiO 2Excessive (Ba, Sr) TiO 3The preparation of mixed phase powder
A. with BaCO 3, SrCO 3And TiO 2Be raw material, adopt solid reaction process, respectively at 1100 ℃, 1200 ℃ synthetic BaTiO 3(being called for short BT), SrTiO 3(being called for short ST) powder;
B. the back of above-mentioned synthetic good BT and ST powder porphyrize being sieved takes by weighing BT and ST powder according to the ratio of mol ratio BT: ST=3:1, with both mixing; Again according to weight ratio TiO 2: (BT+ST)=1～2% take by weighing TiO 2Powder adds in BT and the ST powder mix and fully mixes, and obtains TiO 2Excessive (Ba, Sr) TiO 3The mixed phase powder;
(B), TiO 2Excessive (Ba, Sr) TiO 3The preparation of mixed phase biscuit
A. with above-mentioned TiO 2Excessive (Ba, Sr) TiO 3The mixed phase powder carries out granulation, and is dry-pressing formed, depresses to disk shape sample at static pressure such as 220MPa then;
B. utilize the ice-bath ultrasonic legal system to be equipped with Ba 0.75Sr 0.25TiO 3Colloidal sol; Take by weighing the Ba (OH) of 0.03mol 28H 2The SrAc of O, 0.01mol 2Mix extremely clarification of ultrasonic dissolution under the room temperature of back with 16ml HAc; The benzene that adds the alcohol of positive four butyl esters of metatitanic acid, 12ml of 0.04mol and 5ml in another clean beaker mixes, ultrasonic dissolution is to clarification; Two portions of ultrasonic clear liquors are mixed, carry out ice-bath ultrasonic, reach clear, get Ba 0.75Sr 0.25TiO 3Colloidal sol;
C. disk shape sample is put into the above-mentioned Ba for preparing 0.75Sr 0.25TiO 3Vacuumize in the colloidal sol and ooze
The saturating processing, 700 ℃ of pre-burnings make TiO then 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit;
(C), the preparation of high-performance BST pottery
With above-mentioned pre-burned TiO 2Excessive (Ba, Sr) TiO 3The mixed phase biscuit obtains BST pottery fine and close, that have high tuning rate, high-temperature stability at 1250 ℃～1280 ℃ sintering temperatures.
CN2013101412803A 2013-04-23 2013-04-23 A method for preparing high dielectric tuning ceramic (Ba, sr) TiO3with excessive TiO2 Pending CN103232236A (en)

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Publication number Priority date Publication date Assignee Title
CN105218088A (en) * 2015-09-30 2016-01-06 江苏科技大学 A kind of barium-strontium titanate-based dielectric medium porcelain of nonstoichiometry and preparation method
CN106145934A (en) * 2016-06-12 2016-11-23 上海大学 A kind of microwave-tuned with (Ba, Sr) TiO3ba4ti13o30the preparation method of composite ceramics
CN106946566A (en) * 2017-03-23 2017-07-14 西北工业大学 A kind of preparation method of sheet barium-strontium titanate powder material
CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105218088A (en) * 2015-09-30 2016-01-06 江苏科技大学 A kind of barium-strontium titanate-based dielectric medium porcelain of nonstoichiometry and preparation method
CN106145934A (en) * 2016-06-12 2016-11-23 上海大学 A kind of microwave-tuned with (Ba, Sr) TiO3ba4ti13o30the preparation method of composite ceramics
CN106946566A (en) * 2017-03-23 2017-07-14 西北工业大学 A kind of preparation method of sheet barium-strontium titanate powder material
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CN113860867A (en) * 2021-10-11 2021-12-31 天津大学 Barium titanate-based dielectric ceramic material with high tuning rate and preparation method thereof

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Application publication date: 20130807