CN103708826A - Low dielectric-loss barium strontium titanate pyroelectric ceramic and preparation method thereof - Google Patents
Low dielectric-loss barium strontium titanate pyroelectric ceramic and preparation method thereof Download PDFInfo
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- CN103708826A CN103708826A CN201310729235.XA CN201310729235A CN103708826A CN 103708826 A CN103708826 A CN 103708826A CN 201310729235 A CN201310729235 A CN 201310729235A CN 103708826 A CN103708826 A CN 103708826A
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Abstract
The invention relates to a low dielectric-loss barium strontium titanate pyroelectric ceramic and a preparation method thereof. Chemical constitution of the barium strontium titanate pyroelectric ceramic prepared by the method disclosed by the invention is (Ba1-a-bSra)1-xLaxTi1-bAbO3, wherein x is not less than 0.001 and not greater than 0.01, a is greater than 0 and less than 1, b is not less than 0 and not greater than 0.01, (a+b) is less than 1; A is selected from Mn, Fe, Cu, K, Na, Al and Mg. BST (Barium Strontium Titanate) pyroelectric ceramic disclosed by the invention has small dielectric-loss which can be less than 0.5% (zero-bias fields), is high in sample purity, high in performance, good in uniformity, and capable of satisfying requirements of manufacturing an un-freezing infrared coal plane device, so that a problem that the BST pyroelectric ceramic is great in dielectric-loss is effectively solved.
Description
Technical field
The invention belongs to field of inorganic material preparing technology, be specifically related to pyroelectric ceramic material technical field, a kind of low-dielectric loss strontium-barium titanate pyroelectric ceramics and preparation method thereof is provided.
Background technology
Strontium-barium titanate (Ba
xsr
1-xtiO
3(0<x<1), BST) Curie temperature is adjustable, specific inductivity is high, pyroelectric coefficient high owing to having for stupalith, becomes important candidate material for thermoelectric type non-refrigerating infrared focal plane.
When making non-refrigerating infrared focal plane device, what BST pyroelectric ceramics adopted is novel dielectric operating mode, needs external dc bias field, to obtain the pyroelectric property needing.And after additional direct current biasing electric field, if the dielectric loss of BST pottery is high, easily cause that electrical insulation capability is poor, specific conductivity is high, and make the leakage current of BST pottery excessive, cannot use.In addition, in evaluating infrared focal plane device, detectivity figure of merit F
dvery important parameter, and F
dwith the dielectric loss of BST pottery closely related (formula is as follows):
Wherein p is pyroelectric coefficient, C
vfor specific heat capacity, ε is specific inductivity, and tan δ is dielectric loss;
Dielectric loss is lower, F
dhigher, the performance of device is better.Therefore, also require BST pottery to there is low-dielectric loss.
Yet, generally, the dielectric loss of pure BST pottery is higher, dielectric loss under Curie temperature is generally more than 1%, how effectively to reduce the dielectric loss of BST pottery, making BST pyroelectric ceramics meet the requirement of making non-refrigerating infrared focal plane device, is a technical bottleneck in current BST pyroelectric ceramics research.
Summary of the invention
Problem in the face of prior art exists, the invention provides a kind of low-dielectric loss BST pyroelectric ceramics and preparation method thereof, to meet the requirement of current non-refrigerating infrared focal plane device to BST material.
At this, first the present invention provides a kind of low-dielectric loss strontium-barium titanate pyroelectric ceramics, and its chemical constitution is (Ba
1-a- bsr
a)
1-xla
xti
1-ba
bo
3, 0.001≤x≤0.01 wherein, 0<a<1,0≤b≤0.01, a+b<1, A is selected from Mn, Fe, Cu, K, Na, Al, Mg.
Preferably, described low-dielectric loss strontium-barium titanate pyroelectric ceramics is at zero inclined to one side dielectric loss≤0.5% at Curie temperature place after the match.
BST pyroelectric ceramics dielectric loss of the present invention is little, can reach (zero inclined to one side) below 0.5%, and sample purity is high, performance is high, good uniformity, can meet the requirement of making non-refrigerating infrared focal plane device, effectively solved the large problem of BST ceramic dielectric loss.
Again, the present invention also provides a kind of preparation method of above-mentioned low-dielectric loss strontium-barium titanate pyroelectric ceramics, comprising:
(1) according to stoichiometric ratio, take raw material BaCO
3, SrCO
3, TiO
2, La
2o
3and the oxide compound of A and/or the carbonate of A, adopt wet ball grinding technique to mix, after oven dry, by the weight of described raw material, add the deionized water of 4～10wt% to carry out briquetting, under air atmosphere, at 1000～1200 ℃, be incubated 1～3 hour and make strontium-barium titanate piece; Then to gained strontium-barium titanate piece pulverize, sieving makes (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder;
(2) gained (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder adopts wet ball grinding technique to mix, and adds the binding agent of specified amount after oven dry, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal make strontium-barium titanate base substrate; And
(3) gained strontium-barium titanate base substrate under oxygen atmosphere in the time of 1350～1450 ℃ sintering make described low-dielectric loss barium-strontium titanate ceramic.
Preparation method of the present invention have technique simple, without specific installation, low cost and other advantages, be applicable to large-scale production, can meet industrialization demand.
Preferably, in step (1), wet ball grinding processing condition can be: the mass ratio of raw material, ball-milling medium and deionized water is 1:(1.0～2.0): (1.0～1.5), Ball-milling Time is 12～26 hours, described ball-milling medium is agate ball.
Preferably, in step (1), cross 40 mesh sieves and make (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder.
Preferably, in step (2), wet ball grinding processing condition can be: (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3the mass ratio of powder, ball-milling medium and deionized water is 1:(1.5～2.0): (0.5～1.0), Ball-milling Time is 24～48 hours, described ball-milling medium is agate ball.
Preferably, in step (2), described binding agent is that mass concentration can be 2～5% polyvinyl alcohol solution, and the add-on of described binding agent can be (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
32～5% of powder quality.
Preferably, in step (2), the time of described ageing can be 22～26 hours, and the temperature of described plastic removal can be 750～850 ℃.
Preferably, in step (3), the processing condition of described sintering can be: the speed with 1～4 ℃/min heats up, logical oxygen in sintering process, oxygen flow is 1～3L/mi, when being warming up to 1350～1450 ℃, be incubated 1～5 hour, then cool to room temperature with the furnace, close oxygen.
The present invention has solved the high problem of pure BST ceramic dielectric loss effectively, and preparation method is simple, the cycle is short, cost is low, is applicable to large-scale production, can meet the needs of practical application, has broad application prospects.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the low-dielectric loss BST pyroelectric ceramics that makes of embodiment 1 after surface finish, thermal etching;
Fig. 2 is low-dielectric loss BST pyroelectric ceramics specific inductivity and the dielectric loss variation with temperature graphic representation under zero electric field that embodiment 1 makes;
Fig. 3 is low-dielectric loss BST pyroelectric ceramics specific inductivity and the dielectric loss variation with temperature graphic representation under additional direct current biasing electric field (850V/mm) that embodiment 1 makes;
Fig. 4 is that the BST pyroelectric ceramics that comparative example makes is not adding specific inductivity and dielectric loss variation with temperature graphic representation under DC electric field.
Embodiment
Below provide embodiment and further illustrate by reference to the accompanying drawings the present invention, should be understood that following embodiment is only for the present invention is described, and unrestricted the present invention.
Preparation method provided by the invention can comprise the steps:
First according to general formula (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3, 0.001≤x≤0.01 wherein, 0<a<1,0≤b≤0.01, a+b<1, A is selected from the BaCO that Mn, Fe, Cu, K, Na, Al, Mg take stoichiometric ratio
3, SrCO
3, TiO
2, La
2o
3and the oxide compound of A and/or the material powders such as carbonate of A.Material powder mixes all powders by wet ball grinding technique.Wet ball grinding processing condition can be: the mass ratio of material powder, ball-milling medium and deionized water can be 1:(1.0～2.0): (1.0～1.5), Ball-milling Time is 12～26 hours, described ball-milling medium can adopt agate ball.
After oven dry, add deionized water to carry out briquetting, synthetic in air, synthesis temperature can be 1000～1200 ℃, and soaking time can be 1～3 hour, obtains BST piece.The add-on of deionized water can be 4～10wt% of material powder.
The BST piece obtaining is pulverized, is sieved (for example 40 mesh sieves) make (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder.
Gained (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder mixes powder by wet ball grinding technique, and wet ball grinding processing condition can be: (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3the mass ratio of powder, ball-milling medium and deionized water can be 1:(1.5～2.0): (0.5～1.0), Ball-milling Time is 24～48 hours, described ball-milling medium can be agate ball.
Discharging post-drying, adds a certain amount of binding agent, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal, makes BST idiosome.It is 2%～5% polyvinyl alcohol (PVA) solution that described binding agent can be mass concentration, and the add-on of PVA solution can be 2%～5% of BST powder quality.The time of described ageing can be 22～26 hours.The temperature of described plastic removal can be 750～850 ℃.
The BST base substrate obtaining is carried out to sintering under oxygen atmosphere, sintering process conditions can be: the speed with 1～4 ℃/min heats up, logical oxygen in sintering process, oxygen flow is 1～3L/mi, when being warming up to 1350～1450 ℃, be incubated 1～5 hour, then cool to room temperature with the furnace, close oxygen, obtain low-dielectric loss BST pottery.
The sample sintering is processed into the size needing, ultrasonic cleaning, silk screen printing silver slurry, dries, and at 700 ℃, is incubated 30 minutes, tests dielectric and the pyroelectric property of sample under direct current (DC) bias.Fig. 1 is the stereoscan photograph of example BST pyroelectric ceramics of the present invention after surface finish, thermal etching.As seen from Figure 1: the pore of pottery is few, and density is very high, and grain-size is less.Fig. 2 is that example BST pyroelectric ceramics of the present invention is not adding specific inductivity and dielectric loss variation with temperature graphic representation under DC electric field, as seen from Figure 2: the Curie temperature of pottery is near room temperature, and specific inductivity is 10
3the order of magnitude, the dielectric loss under Curie temperature is 0.45%.Fig. 3 is BST pyroelectric ceramics of the present invention (850V/mm) specific inductivity and dielectric loss variation with temperature graphic representation under applying direct current electric field, as seen from Figure 3: the Curie temperature of pottery is than high under zero electric field, but still near room temperature, dielectric loss is lower, and the dielectric loss under Curie temperature only has 0.35%.Visible, it is low (under zero electric field that the BST pyroelectric ceramics that adopts the present invention to prepare has dielectric loss, the dielectric loss at Curie temperature place is no more than 0.45%), and microtexture is excellent, as few in pore, density is high, grain-size is tiny evenly, can meet the requirement of making non-refrigerating infrared focal plane device.The present invention has solved the higher difficult problem of BST ceramic dielectric loss effectively, and preparation method is simple, the cycle is short, cost is low, is applicable to large-scale production, can meet the needs of practical application.
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., those skilled in the art can do in suitable scope and be selected by explanation herein the temperature that following example is concrete, time, charging capacity etc. are only also examples in OK range,, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
Take material powder BaCO
3(801.87g), SrCO
3(288.57g), TiO
2(480.64g) and La
2o
3(6.85g), and 0.69g MnCO
3powder, mixes all powders by wet ball grinding technique; The mass ratio of material, ball-milling medium and deionized water is 1:1.5:1.2, and Ball-milling Time is 24 hours, and ball-milling medium is agate ball.
Abrasive material is dried, add the deionized water of total powder quality 4%, briquetting, synthetic in air, synthesis temperature is 1150 ℃, soaking time is 2 hours, obtains BST piece; Pulverize, cross 40 mesh sieves, by wet ball grinding technique, powder is mixed; The mass ratio of material, ball-milling medium and deionized water is 1:2.0:0.8, and Ball-milling Time is 48 hours, and ball-milling medium is agate ball.
Dry, add PVA solution as binding agent, granulation, ageing 24 hours, sieves, and carries out isostatic pressing after precompressed, and biscuit, at 800 ℃ of plastic removals, makes BST base substrate; By BST base substrate sintering under oxygen, the condition of sintering is: the speed with 2.0 ℃/min heats up; And logical oxygen, oxygen flow is 2L/min; When being warming up to 1350 ℃, be incubated 5 hours; Be cooled to room temperature, close oxygen.
The sample sintering is processed into the size needing, ultrasonic cleaning, silk screen printing silver slurry, dries, and at 700 ℃, is incubated 30 minutes, tests dielectric and the pyroelectric property of sample under direct current (DC) bias.
Fig. 1 is the stereoscan photograph of the BST pyroelectric ceramics that makes of the present embodiment after surface finish, thermal etching.As seen from Figure 1: the pore of pottery is few, and density is very high, and grain-size is less.
Fig. 2 is that the BST pyroelectric ceramics that the present embodiment makes is not adding specific inductivity and dielectric loss variation with temperature graphic representation under DC electric field, as seen from Figure 2: the Curie temperature of pottery is near room temperature, and specific inductivity is 10
3the order of magnitude, the dielectric loss under Curie temperature is 0.45%, compares in following comparative example and mixes the BST pottery of Y in proportion, only has an appointment 1/5.
Fig. 3 is BST pyroelectric ceramics (850V/mm) specific inductivity and the dielectric loss variation with temperature graphic representation under applying direct current electric field that the present embodiment makes, as seen from Figure 3: the Curie temperature of pottery is than high under zero electric field, but still near room temperature, dielectric loss is lower, and the dielectric loss under Curie temperature only has 0.35%.
Comparative example
Take material powder BaCO
3(801.87g), SrCO
3(288.57g), TiO
2(480.64g) and Y
2o
3(4.74g), and 0.69g MnCO
3powder, mixes all powders by wet ball grinding technique; The mass ratio of material, ball-milling medium and deionized water is 1:1.5:1.2, and Ball-milling Time is 24 hours, and ball-milling medium is agate ball.
Abrasive material is dried, add the deionized water of total powder quality 4%, briquetting, synthetic in air, synthesis temperature is 1150 ℃, soaking time is 2 hours, obtains BST piece; Pulverize, cross 40 mesh sieves, by wet ball grinding technique, powder is mixed; The mass ratio of material, ball-milling medium and deionized water is 1:2.0:0.8, and Ball-milling Time is 48 hours, and ball-milling medium is agate ball.
Dry, add PVA solution as binding agent, granulation, ageing 24 hours, sieves, and carries out isostatic pressing after precompressed, and biscuit, at 800 ℃ of plastic removals, makes BST base substrate; By BST base substrate sintering under oxygen, the condition of sintering is: the speed with 2.0 ℃/min heats up; And logical oxygen, oxygen flow is 2L/min; When being warming up to 1350 ℃, be incubated 5 hours; Be cooled to room temperature, close oxygen.
The sample sintering is processed into the size needing, ultrasonic cleaning, silk screen printing silver slurry, dries, and at 700 ℃, is incubated 30 minutes, tests dielectric and the pyroelectric property of sample under direct current (DC) bias.
Fig. 4 is not adding specific inductivity and dielectric loss variation with temperature graphic representation under DC electric field for the BST pyroelectric ceramics that this comparative example makes, as seen from Figure 4: the Curie temperature of pottery is near room temperature, and specific inductivity is 10
4the order of magnitude, the dielectric loss under Curie temperature is 2.37%.
In sum, it is low (under zero electric field that the BST pyroelectric ceramics that adopts the present invention to prepare has dielectric loss, the dielectric loss at Curie temperature place is no more than 0.45%), and microtexture is excellent, as few in pore, density is high, grain-size is tiny evenly, can meet the requirement of making non-refrigerating infrared focal plane device.
Industrial applicability: the BST pyroelectric ceramics that adopts the present invention to prepare has low-dielectric loss, can meet the requirement of making non-refrigerating infrared focal plane device.The present invention has solved the higher difficult problem of BST ceramic dielectric loss effectively, and preparation method is simple, the cycle is short, cost is low, is applicable to large-scale production, can meet the needs of practical application.
Claims (9)
1. a low-dielectric loss strontium-barium titanate pyroelectric ceramics, is characterized in that, its chemical constitution is (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3, 0.001≤x≤0.01 wherein, 0<a<1,0≤b≤0.01, a+b<1, A is selected from Mn, Fe, Cu, K, Na, Al, Mg.
2. low-dielectric loss strontium-barium titanate pyroelectric ceramics according to claim 1, is characterized in that, described low-dielectric loss strontium-barium titanate pyroelectric ceramics is at zero inclined to one side dielectric loss≤0.5% at Curie temperature place after the match.
3. a preparation method for low-dielectric loss strontium-barium titanate pyroelectric ceramics according to claim 1 and 2, is characterized in that, comprising:
(1) according to stoichiometric ratio, take raw material BaCO
3, SrCO
3, TiO
2, La
2o
3and the oxide compound of A and/or the carbonate of A, adopt wet ball grinding technique to mix, after oven dry, by the weight of described raw material, add the deionized water of 4～10wt% to carry out briquetting, under air atmosphere, at 1000～1200 ℃, be incubated 1～3 hour and make strontium-barium titanate piece; Then to gained strontium-barium titanate piece pulverize, sieving makes (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder;
(2) gained (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder adopts wet ball grinding technique to mix, and adds the binding agent of specified amount after oven dry, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal make strontium-barium titanate base substrate; And
(3) gained strontium-barium titanate base substrate under oxygen atmosphere in the time of 1350～1450 ℃ sintering make described low-dielectric loss barium-strontium titanate ceramic.
4. preparation method according to claim 3, it is characterized in that, in step (1), wet ball grinding processing condition are: the mass ratio of raw material, ball-milling medium and deionized water is 1:(1.0～2.0): (1.0～1.5), Ball-milling Time is 12 ~ 26 hours, and described ball-milling medium is agate ball.
5. according to the preparation method described in claim 3 or 4, it is characterized in that, in step (1), cross 40 mesh sieves and make (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3powder.
6. according to the preparation method described in any one in claim 3～5, it is characterized in that, in step (2), wet ball grinding processing condition are: (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
3the mass ratio of powder, ball-milling medium and deionized water is 1:(1.5～2.0): (0.5～1.0), Ball-milling Time is 24～48 hours, described ball-milling medium is agate ball.
7. according to the preparation method described in any one in claim 3～6, it is characterized in that, in step (2), described binding agent is that mass concentration is 2～5% polyvinyl alcohol solution, and the add-on of described binding agent is (Ba
1-a-bsr
a)
1-xla
xti
1-ba
bo
32～5% of powder quality.
8. according to the preparation method described in any one in claim 3～7, it is characterized in that, in step (2), the time of described ageing is 22～26 hours, and the temperature of described plastic removal is 750～850 ℃.
9. according to the preparation method described in any one in claim 3～8, it is characterized in that, in step (3), the processing condition of described sintering are: the speed with 1～4 ℃/min heats up, logical oxygen in sintering process, and oxygen flow is 1～3L/mi, when being warming up to 1350～1450 ℃, be incubated 1 ~ 5 hour, then cool to room temperature with the furnace, close oxygen.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710170A (en) * | 2015-02-12 | 2015-06-17 | 中国科学院上海硅酸盐研究所 | Barium strontium titanate pyroelectric ceramic prepared from uniform fine grains and preparation method thereof |
| CN106588006A (en) * | 2016-12-15 | 2017-04-26 | 中国工程物理研究院材料研究所 | High-dielectric property BST (Barium Strontium Titanate), preparation method thereof and dielectric ceramic prepared by adopting same |
| CN106747415A (en) * | 2017-03-03 | 2017-05-31 | 华东理工大学 | A kind of preparation of low-dielectric loss calcium titanate ceramics |
| CN115845829A (en) * | 2022-11-24 | 2023-03-28 | 中南大学 | Oriented porous piezoelectric ceramic catalyst and preparation method and application thereof |
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| CN1511124A (en) * | 2001-08-09 | 2004-07-07 | 大里齐 | Microwave dielectric composite composition |
| CN101844919A (en) * | 2010-06-03 | 2010-09-29 | 西北工业大学 | Composite barium strontium titanate ceramics and preparation method thereof |
| CN102976748A (en) * | 2012-12-28 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | High-density barium strontium titanate ceramic and preparation method thereof |
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2013
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511124A (en) * | 2001-08-09 | 2004-07-07 | 大里齐 | Microwave dielectric composite composition |
| CN101844919A (en) * | 2010-06-03 | 2010-09-29 | 西北工业大学 | Composite barium strontium titanate ceramics and preparation method thereof |
| CN102976748A (en) * | 2012-12-28 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | High-density barium strontium titanate ceramic and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710170A (en) * | 2015-02-12 | 2015-06-17 | 中国科学院上海硅酸盐研究所 | Barium strontium titanate pyroelectric ceramic prepared from uniform fine grains and preparation method thereof |
| CN106588006A (en) * | 2016-12-15 | 2017-04-26 | 中国工程物理研究院材料研究所 | High-dielectric property BST (Barium Strontium Titanate), preparation method thereof and dielectric ceramic prepared by adopting same |
| CN106588006B (en) * | 2016-12-15 | 2019-11-12 | 中国工程物理研究院材料研究所 | A kind of high dielectric property barium strontium titanate, preparation method and the dielectric ceramic using its preparation |
| CN106747415A (en) * | 2017-03-03 | 2017-05-31 | 华东理工大学 | A kind of preparation of low-dielectric loss calcium titanate ceramics |
| CN115845829A (en) * | 2022-11-24 | 2023-03-28 | 中南大学 | Oriented porous piezoelectric ceramic catalyst and preparation method and application thereof |
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Application publication date: 20140409 |