CN102976748B - High-density barium strontium titanate ceramic and preparation method thereof - Google Patents
High-density barium strontium titanate ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to high-density barium strontium titanate ceramic and a preparation method thereof. The high-density barium strontium titanate ceramic comprises (Ba1-a-bSraCab)1-cAcTi1-dBdO3 powder and ZnO powder, wherein a is greater than 0 and less than 1; b is greater than or equal to 0 and is less than or equal to 0.3; c is greater than or equal to 0 and is less than or equal to 0.03; d is greater than or equal to 0 and is less than or equal to 0.01; A is selected from Y, La and Sm; B is selected from Mn, Fe, Cu, K, Na, Al and Mg; and the mass of the ZnO powder is 2 to 3 percent of that of the (Ba1-a-bSraCab)1-cAcTi1-dBdO3 powder. The BST (barium strontium titanate) pyroelectric ceramic disclosed by the invention has high density and excellent electrical property and can meet the requirement for manufacturing an uncooled infrared focal plane device.
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 high fine and close barium-strontium titanate ceramic and preparation method thereof is provided, especially by adding sintering agent, prepare the method for high fine and close barium strontium titanate pyroelectric ceramics.
Background technology
Barium strontium titanate (Ba
xsr
1-xtiO
3(0<x<1), BST) Curie temperature is adjustable, dielectric constant is high, dielectric loss is low, pyroelectric coefficient high owing to having for ceramic material, becomes important candidate material for thermoelectric type non-refrigerating infrared focal plane.
While using BST pyroelectric ceramics to make non-refrigerating infrared focal plane device, conventionally need to be thinned to below 30 microns, this is that in the time of can making to absorb same infrared radiation heat due to thin ceramic wafers, variations in temperature is larger, thereby can improve the sensitivity of device, therefore BST pottery must have very high density, could meet the requirement of attenuate processing; In addition, during due to the work of BST pottery, need extra electric field, if the density of BST pottery is lower, there is increased number of stomata, easily in the course of processing, introduce the poor impurity of insulation property, cause conducting, make detector have more blind spot until lost efficacy, this also requires BST pottery should have high density.In general, the relative density of BST pottery should reach more than 96%.
Yet, because BST pottery exists the feature that sintering reaches high-compactness that is difficult to, generally, BST pottery can only be sintered to the density below 96%, how effectively to improve the density 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.
CN102030524A discloses a kind of solid-state pulse forming line energy storage dielectric material, the Ba that it forms and proportioning is 70～90wt%
0.4sr
0.6tiO
3with the nano-MgO of 10～30 problem %, can so that the density of barium strontium titanate bring up to more than 98.5%.
Again, CN101302100B discloses a kind of method of preparing strontium titanate and barium titanate electronic function ceramic using laser material, and it adopts CO
2laser carries out sintering to improve the density of barium strontium titanate.
Summary of the invention
In the face of the problem that prior art exists, the inventor provides fine and close barium-strontium titanate ceramic of a kind of new height 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 kind of a high fine and close barium-strontium titanate ceramic, comprises (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3powder and ZnO powder, 0<a<1 wherein, 0≤b≤0.3,0≤c≤0.03,0≤d≤0.01, A is selected from Y, La, Sm, and B is selected from Mn, Fe, Cu, K, Na, Al, Mg, and the quality of described ZnO powder is (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
32～3% of the quality of powder.
BST pyroelectric ceramics of the present invention has high density, and electrical property is good, can meet the requirement of making non-refrigerating infrared focal plane device.
Preferably, density >=98.5% of the fine and close barium-strontium titanate ceramic of described height.
On the other hand, the present invention also provides the preparation method of the fine and close barium-strontium titanate ceramic of a kind of above-mentioned height, comprising:
Step a: at described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3in powder, add the ZnO powder of 2～3wt%, adopt wet ball grinding technique to mix, after oven dry, add the binding agent of ormal weight, through granulation, ageing, sieve after precompressed again, isostatic compaction, plastic removal make barium strontium titanate base substrate; And
Step b: gained barium strontium titanate base substrate under oxygen atmosphere in the time of 1350～1450 ℃ sintering make the fine and close barium-strontium titanate ceramic of described height.
Preferably, in described step a, the mass ratio of powder and ball-milling medium and deionized water can be 1:(1.5～2.0): (0.5～1.0), Ball-milling Time can be 24～48 hours, and described ball-milling medium can be agate ball.
Preferably, in described step a, it is 2～5% poly-vinyl alcohol solution that described binding agent can be mass concentration, and the addition of described binding agent can be (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
32%～5% of powder quality.
Preferably, in described step a, the time of described ageing can be 22～26 hours, and the temperature of described plastic removal can be 750～850 ℃.
Preferably, in described step b, the speed intensification with 1～4 ℃/min starts logical oxygen when being warming up to 800～1000 ℃, and oxygen flow is 1～3L/min; When being warming up to 1350～1450 ℃, be incubated 1 ~ 5 hour, then cool to room temperature with the furnace, close oxygen.
Again, preferably, (the Ba that the present invention is used
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3powder is prepared by following method:
According to stoichiometric proportion, take BaCO
3, SrCO
3, CaCO
3, TiO
2and the carbonate of the oxide of A, B and/or A, B, adopt wet ball grinding technique to mix;
After oven dry, add the deionized water of 4～10wt% to carry out briquetting, under air atmosphere, at 1000 ~ 1200 ℃, be incubated 1～3 hour and make barium strontium titanate piece; And
Gained barium strontium titanate piece is pulverized, sieved.
Preferably, at described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3in the preparation process of powder, wet ball grinding process conditions are: the mass ratio of material and 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, described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3powder was the powder of 40 mesh sieves.
The present invention has effectively solved BST pottery and has been difficult to be sintered to a high fine and close difficult problem, 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 fine and close BST pyroelectric ceramics of the height that makes of embodiment 1 after surface finish, hot corrosion;
Fig. 2 is the fine and close BST pyroelectric ceramics of height dielectric constant and the dielectric loss variation with temperature curve chart under applying direct current electric field that embodiment 1 makes;
Fig. 3 is the pyroelectric coefficient variation with temperature curve chart that the fine and close BST pyroelectric ceramics of the height that makes of embodiment 1 adopts Quasi-static Method test under applying direct current electric field.
Embodiment
Below provide embodiment and further illustrate by reference to the accompanying drawings the present invention, should be understood that following execution mode is only for the present invention is described, and unrestricted the present invention.
Preparation method provided by the invention can comprise the steps:
1) first according to general formula (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3(0<a<1,0≤b≤0.3,0≤c≤0.03,0≤d≤0.01, A is selected from Y, La, Sm, B is selected from Mn, Fe, Cu, K, Na, Al, Mg) take the material powders such as barium source, strontium source, calcium source, titanium source and doped chemical (A, B) source of stoichiometric proportion, barium source, strontium source, calcium source, titanium source can adopt respectively BaCO
3, SrCO
3, CaCO
3and TiO
2powder, A, B source can adopt its oxide or carbonate, for example Y
2o
3, MnCO
3powder.Material powder mixes all powders by wet ball grinding technique.
2) dry rear briquetting, synthetic in air, synthesis temperature can be 1000～1200 ℃, and temperature retention time can be 1 ~ 3 hour, obtains BST piece.
3) by step 2) the BST piece that obtains pulverizes, sieves, then add sintering agent ZnO, by wet ball grinding technique, powder is mixed.
4) discharging post-drying, adds a certain amount of binding agent, through granulation, ageing, sieve after precompressed again, isostatic compaction, plastic removal, makes BST idiosome.
5) by step 4) the BST base substrate that obtains carries out sintering under oxygen atmosphere, and sintering process conditions can be: the speed with 1～4 ℃/min heats up, and starts logical oxygen when being warming up to 800～1000 ℃, and oxygen flow is 1～3L/min; When being warming up to 1350～1450 ℃, be incubated 1 ~ 5 hour; Cool to room temperature with the furnace, close oxygen, obtain high fine and close BST pottery.
In above-mentioned steps 1) in wet ball grinding process conditions can be: the mass ratio of material and 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.
Step 2) in: the deionization that adds total powder 4%～10% quality after oven dry, before briquetting.
Step 3) in: BST powder is crossed 40 mesh sieves before carrying out wet ball grinding.
Step 3) sintering agent in is ZnO, and addition is the 2wt% ~ 3wt% of BST powder.
Step c) in, wet ball grinding process conditions can be: the mass ratio of material and 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.
Step 4) it is 2%～5% polyvinyl alcohol (PVA) solution that the binding agent described in can be mass concentration, and the addition of PVA solution can be 2%～5% of BST powder quality.
Step 4) digestion time in can be 22～26 hours.
Step 4) the plastic removal temperature in can be 750～850 ℃.
Through test, learn, the present invention compared with prior art, has following beneficial effect:
1) BST pyroelectric ceramics density of the present invention is high, can reach more than 98%, 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 problem that BST pottery is difficult to sinter to high-compactness;
2) preparation method of the present invention have technique simple, without special installation, low cost and other advantages, be applicable to large-scale production, can meet industrialization demand.
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, inventory etc. are only also examples in OK range,, and do not really want to be defined in the below concrete numerical value of example.Again, although below only not contain Ca, the Preparation Example of the barium-strontium titanate ceramic of codope Y, Mn, should be understood that above-mentioned chemical composition ((Ba
1-a-bsr
aca
b)
1- ca
cti
1-db
do
3) limit other containing the barium-strontium titanate ceramic of Ca, the barium-strontium titanate ceramic of the doped chemical that undopes, and/or multi-element doping barium-strontium titanate ceramic can be prepared by similar method.
Embodiment 1
Take BaCO
3(796.3g), SrCO
3(292.7g) TiO
2(480.6g) powder, and add a small amount of Y
2o
3(4.7g), MnCO
3(0.7g) powder, 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 ℃, temperature retention time is 2 hours, obtains BST piece; Pulverize, cross 40 mesh sieves;
The ZnO powder that adds 2.7wt%, mixes powder by wet ball grinding technique, and 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 compaction 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; When being warming up to 800 ℃, start logical oxygen, oxygen flow is 2L/min; When being warming up to 1350 ℃, be incubated 5 hours; Be cooled to room temperature, close oxygen, make high fine and close 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 the fine and close BST pyroelectric ceramics of the height that makes of the present embodiment after surface finish, hot corrosion.As seen from Figure 1: the pore of pottery is few, and density is very high, and the relative density measuring through Archimedes's method is 98.62%.
Fig. 2 is the fine and close BST pyroelectric ceramics of height dielectric constant and the dielectric loss variation with temperature curve chart under applying direct current electric field that the present embodiment makes, as seen from Figure 2: the Curie temperature of pottery is near room temperature, and dielectric constant is 10
4the order of magnitude, along with the increase of electric field, Curie temperature is to high-temperature mobile, and dielectric constant declines, and dielectric loss reduces, and under 850V/mm electric field, the dielectric loss under 25 ° of C of room temperature is low to moderate 0.67%.
Fig. 3 is that the fine and close BST pyroelectric ceramics of height that the present embodiment makes adopts the pyroelectric coefficient of Quasi-static Method test with the change curve of temperature and applying direct current electric field, as seen from Figure 3: with temperature, increase, pyroelectric coefficient first increases afterwards and reduces, and pyroelectric coefficient peak value is 20.6 * 10
-8ccm
-2k
-1.
Industrial applicability: the BST pyroelectric ceramics that adopts the present invention to prepare has advantages of density high (relative density>=98.5%), and electrical property is excellent, as dielectric constant large (10
4the order of magnitude), dielectric loss little (< 1%), pyroelectric property is high, when 850V/mm bias field, its pyroelectric coefficient can reach 20.6 * 10
-8ccm
-2k
-1, can meet the requirement of making non-refrigerating infrared focal plane device.The present invention has solved the difficult problem that BST pottery is difficult to sinter to high-compactness 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 (7)
1. a preparation method for high fine and close barium-strontium titanate ceramic, is characterized in that, the fine and close barium-strontium titanate ceramic of described height comprises (Ba
1-a- bsr
aca
b)
1-ca
cti
1-db
do
3powder and ZnO powder, 0<a<1 wherein, 0≤b≤0.3,0≤c≤0.03,0≤d≤0.01, A is selected from Y, La, Sm, and B is selected from Mn, Fe, Cu, K, Na, Al, Mg, and the quality of described ZnO powder is (Ba
1- a-bsr
aca
b)
1-ca
cti
1-db
do
32～3% of powder quality, described preparation method comprises:
Step a: at described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3in powder, add the ZnO powder of 2～3wt%, adopt wet ball grinding technique to mix, after oven dry, add the binding agent of ormal weight, through granulation, ageing, sieve after precompressed again, isostatic compaction, plastic removal make barium strontium titanate base substrate; And
Step b: gained barium strontium titanate base substrate under oxygen atmosphere in the time of 1350～1450 ℃ sintering make the fine and close barium-strontium titanate ceramic of described height;
Wherein, in described step b, the speed intensification with 1～4 ℃/min starts logical oxygen when being warming up to 800～1000 ℃, and oxygen flow is 1～3L/min; When being warming up to 1350～1450 ℃, be incubated 1～5 hour, then cool to room temperature with the furnace, close oxygen.
2. preparation method according to claim 1, it is characterized in that, in described step a, the mass ratio of powder and ball-milling medium and deionized water is 1:(1.5～2.0): (0.5～1.0), Ball-milling Time is 24～48 hours, and described ball-milling medium is agate ball.
3. preparation method according to claim 1 and 2, is characterized in that, in described step a, described binding agent is that mass concentration is 2～5% poly-vinyl alcohol solution, and the addition of described binding agent is (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
32%～5% of powder quality.
4. preparation method according to claim 1 and 2, is characterized in that, in described step a, the time of described ageing is 22～26 hours, and the temperature of described plastic removal is 750～850 ℃.
5. preparation method according to claim 1 and 2, is characterized in that, also comprises described (Ba
1-a-bsr
aca
b)
1-ca
cti
1- db
do
3the preparation process of powder:
According to stoichiometric proportion, take BaCO
3, SrCO
3, CaCO
3, TiO
2and the carbonate of the oxide of A, B and/or A, B, adopt wet ball grinding technique to mix;
After oven dry, add the deionized water of 4～10wt% to carry out briquetting, under air atmosphere, at 1000～1200 ℃, be incubated 1～3 hour and make barium strontium titanate piece; And
Gained barium strontium titanate piece is pulverized, sieved.
6. preparation method according to claim 5, is characterized in that, at described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3in the preparation process of powder, wet ball grinding process conditions are: the mass ratio of material and 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.
7. preparation method according to claim 1 and 2, described (Ba
1-a-bsr
aca
b)
1-ca
cti
1-db
do
3powder was the powder of 40 mesh sieves.
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| CN103708826A (en) * | 2013-12-25 | 2014-04-09 | 中国科学院上海硅酸盐研究所 | Low dielectric-loss barium strontium titanate pyroelectric ceramic and preparation method thereof |
| CN104496471A (en) * | 2014-11-26 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | High-Curie-temperature lead-free pyroelectric ceramic material and preparation method thereof |
| 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 |
| CN105461298B (en) * | 2015-12-05 | 2018-01-12 | 浙江大学 | Barium-strontium titanate-based ceramics of a kind of manganese ion aliquot replacement titanium ion high energy storage density and preparation method thereof |
| CN111389242B (en) * | 2020-03-19 | 2022-08-05 | 上海大学 | Cobalt-free anti-CO 2 Poisoned high oxygen-permeable biphase oxygen-permeable membrane material, its preparation method and application |
| CN114262224A (en) * | 2021-11-26 | 2022-04-01 | 西安交通大学 | Composite doped barium strontium titanate ceramic and preparation method thereof |
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Non-Patent Citations (2)
| Title |
|---|
| Dielectric and pyroelectric properties of poled Ba0.6Sr0.3Ca0.1TiO3 ceramics;Sheng Cao et al.;《Phys. Status Solidi A》;20110317;第208卷(第5期);第1127-1131页 * |
| Sheng Cao et al..Dielectric and pyroelectric properties of poled Ba0.6Sr0.3Ca0.1TiO3 ceramics.《Phys. Status Solidi A》.2011,第208卷(第5期),第1127-1131页. * |
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