CN102060527B - Doped and modified barium strontium calcium titanate heat-release pyroelectric ceramic material and preparation method thereof - Google Patents
Doped and modified barium strontium calcium titanate heat-release pyroelectric ceramic material and preparation method thereof Download PDFInfo
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- CN102060527B CN102060527B CN 201010584351 CN201010584351A CN102060527B CN 102060527 B CN102060527 B CN 102060527B CN 201010584351 CN201010584351 CN 201010584351 CN 201010584351 A CN201010584351 A CN 201010584351A CN 102060527 B CN102060527 B CN 102060527B
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Abstract
The invention discloses a doped and modified barium strontium calcium titanate heat-release pyroelectric ceramic material which has the composition formula of (Ba0.6Sr0.3Ca0.1)1-xYxTi0.999Mn0.001O3, wherein x is equal to 0.001 to 0.010. The heat-release pyroelectric ceramic material disclosed in the invention is prepared by adopting a simple solid phase method powder preparing and atmosphere sintering process. The barium strontium calcium titanate pyroelectric ceramic material which is doped and modified by Y and Mn not only has small grain size and large dielectric constant but also has higher pyroelectric performance, can meet the performance requirement for manufacturing a non-refrigerating infrared focal plane device and effectively solves the contradiction between the fine grain sizeand high pyroelectric performance. The preparation method disclosed in the invention has the advantages of simple process, no need of special equipment, low cost, and the like, is suitable for mass production and can meet the industrialized demand.
Description
Technical field
The present invention relates to a kind of barium strontium calcium titanate pyroelectric ceramic material and preparation method thereof, specifically, relate to a kind of barium strontium calcium titanate pyroelectric ceramic material through Y, Mn doping vario-property and preparation method thereof, belong to the pyroelectric ceramic material technical field.
Background technology
Infrared Focal plane Array Technologies comprises two kinds of refrigeration mode and non-refrigeration types, and refrigeration mode is take the low-gap semiconductor Hg-Cd-Te material as representative, and non-refrigeration type comprises thermoelectric type and two kinds of main Types of micrometer bolometer.And the thermoelectric type Infrared Focal plane Array Technologies since need not the refrigeration, response spectrum is wide, and is low in energy consumption, miniaturization, reliability is high, and using the advantage such as have a large capacity and a wide range becomes one of emphasis of current infrared focal plane imaging technical study and application, is widely used at numerous areas.
Pyroelectricity material is one of crucial sensitive material of non-refrigerating infrared focal plane device.And strontium-barium titanate base ceramic material (Ba
xSr
1-xTiO
3, be called for short BST) because its high-k, low-dielectric loss, Curie temperature and dielectric properties are adjustable, with and near ferroelectric para-electric phase transformation high pyroelectric property become one of important candidate material of non-refrigerating infrared focal plane device.
But along with the integrated and degree of miniaturization of focal plane technology is more and more higher, the attenuate of strontium-barium titanate base ceramic material is had higher requirement.When making infrared focal plane detector, pyroelectric ceramic material must be thinned to below tens microns.And the attenuate of stupalith depends primarily on the grain-size of pottery, and grain-size is less, easier attenuate.After but grain-size reduced, its dielectric and pyroelectric property can reduce again, therefore had the contradiction between a fine grain size and the high pyroelectric property here.So, how effectively to avoid the contradiction between fine grain size and the high pyroelectric property, barium-strontium titanate-based pyroelectric ceramic material being satisfied make the requirement of non-refrigerating infrared focal plane performance of devices, is the difficult problem of the solution of needing badly in studying about barium-strontium titanate-based pyroelectric ceramic material at present.
Summary of the invention
The purpose of this invention is to provide a kind of less grain-size that not only has, and has a higher pyroelectric response, can effectively avoid the contradiction between fine grain size and the high pyroelectric property, can satisfy and make non-refrigerating infrared focal plane performance of devices requirement, through barium strontium calcium titanate pyroelectric ceramic material of doping vario-property and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is as follows:
Barium strontium calcium titanate pyroelectric ceramic material through doping vario-property provided by the invention, its composition general formula is: (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3, x=0.001～0.010 wherein.
The preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property provided by the invention comprises following concrete steps:
A) at first according to general formula (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder mixes all powders with wet ball grinding technique;
B) briquetting after the oven dry, synthetic under air atmosphere, synthesis temperature is 1000～1200 ℃, soaking time is 1～3 hour, is consisted of (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder;
C) with step b) obtain consist of (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder pulverize, sieve, with wet ball grinding technique powder is mixed again;
D) oven dry adds binding agent, through granulation, ageing, sieve, moulding, plastic removal step, to make (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Base substrate;
E) with steps d) (the Ba that obtains
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Base substrate carries out sintering under oxygen atmosphere, the processing condition of sintering are: the speed with 1～4 ℃/min heats up; Begin logical oxygen when being warmed up to 800～1000 ℃, oxygen flow is 1～3L/min; When being warmed up to 1400～1450 ℃, be incubated 1～2 hour; Cool to room temperature with the furnace, close oxygen.
The wet ball grinding processing condition of step in a) are recommended as: the mass ratio of ball milling material and ball-milling medium and deionized water is 1: (1.0～2.0): (1.0～1.5), Ball-milling Time is 12～24 hours, and described ball-milling medium is steel ball, zirconium ball or agate ball.
Step b) in: the deionized water of after oven dry, before the briquetting, recommending to add total powder 10% quality.
Step c) in: (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder was recommended 40 mesh sieves before carrying out wet ball grinding.
Step c) the wet ball grinding processing condition in are recommended as: the mass ratio of ball milling 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, and described ball-milling medium is steel ball, zirconium ball or agate ball.
Steps d) in: described binding agent is recommended as polyvinyl alcohol (PVA), and add-on is recommended as 3～6% of powder quality.
Steps d) in: digestion time is recommended as 22～26 hours.
Steps d) in: before moulding, recommended 20 mesh sieves.
Steps d) in: the temperature of plastic removal is recommended as 750～850 ℃.
The present invention after the polishing thermal etching, utilizes the size of its grain-size of scanning electron microscope Observable with sample surfaces; The Machining of Ceramics that sinters is become desired size, ultrasonic cleaning, silk screen printing silver slurry, oven dry 650～750 ℃ of lower insulations 20～40 minutes, namely obtains can be used for (the Ba of electric property assessment
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Ceramics sample.
Learn through test, the present invention compared with prior art has following beneficial effect:
1) barium strontium calcium titanate pyroelectric ceramic material through Y, Mn doping vario-property of the present invention not only has grain-size little (1～3 micron), specific inductivity large (10
4Magnitude), and have higher pyroelectric property, when the 700V/mm bias field, its pyroelectric coefficient can reach (25～35) * 10
-8C/cm
2K surveys the figure of merit and can reach (7～9) * 10
-5Pa
-1/2, can satisfy and make the requirement of non-refrigerating infrared focal plane performance of devices, effectively solved the contradiction between fine grain size and the high pyroelectric property.
2) preparation method of the present invention have technique simple, need not specific installation, low cost and other advantages, be fit to large-scale production, can satisfy the industrialization demand.
Description of drawings
Fig. 1 is the stereoscan photograph of barium strontium calcium titanate pyroelectric ceramic material after surface finish, thermal etching that embodiment 1 makes.
Fig. 2 is the change curve of barium strontium calcium titanate pyroelectric ceramic material dielectric constant with temperature under applying direct current electric field of making of embodiment 1.
Fig. 3 is barium strontium calcium titanate pyroelectric ceramic material dielectric loss variation with temperature graphic representation under applying direct current electric field that embodiment 1 makes.
Fig. 4 is that the barium strontium calcium titanate pyroelectric ceramic material that embodiment 1 makes adopts the pyroelectric coefficient of Quasi-static Method test with the change curve of temperature and applying direct current electric field.
Specific implementation method
The present invention is described in further detail and completely below in conjunction with embodiment.
Embodiment 1
At first according to general formula (Ba
0.6Sr
0.3Ca
0.1)
0.993Y
0.007Ti
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder mixes all powders with wet ball grinding technique; The mass ratio of ball milling material and ball-milling medium and deionized water is 1: 1.5: 1.2, and Ball-milling Time is 18 hours, and described ball-milling medium is steel ball, zirconium ball or agate ball.
Dry, add the deionized water of total powder 10% weight, briquetting, synthetic under air atmosphere, synthesis temperature is 1100 ℃, soaking time is 2 hours, is consisted of (Ba
0.6Sr
0.3Ca
0.1)
0.993Y
0.007Ti
0.999Mn
0.001O
3Powder; Pulverize, cross 40 mesh sieves, with wet ball grinding technique powder is mixed again; The mass ratio of ball milling material and ball-milling medium and deionized water is 1: 1.8: 0.7, and Ball-milling Time is 36 hours, and described ball-milling medium is steel ball, zirconium ball or agate ball.
Oven dry, polyvinyl alcohol (PVA) binding agent of adding powder quality 4.5%, granulation, 20 mesh sieves are crossed in ageing 24 hours, and moulding at 800 ℃ of plastic removals, namely makes (Ba
0.6Sr
0.3Ca
0.1)
0.993Y
0.007Ti
0.999Mn
0.001O
3Base substrate; Base substrate is carried out sintering under oxygen atmosphere, the processing condition of sintering are: the speed with 2.5 ℃/min heats up; Begin logical oxygen when being warmed up to 900 ℃, oxygen flow is 2L/min; When being warmed up to 1400～1450 ℃, be incubated 1～2 hour; Cool to room temperature with the furnace, close oxygen.
Fig. 1 is the stereoscan photograph of barium strontium calcium titanate pyroelectric ceramic material after surface finish, thermal etching that the present embodiment makes, and as seen from Figure 1: the grain-size of pottery is less, between 1～3 μ m.
Fig. 2 is the change curve of barium strontium calcium titanate pyroelectric ceramic material dielectric constant with temperature under applying direct current electric field of making of the present embodiment, and as seen from Figure 2: the Curie temperature of pottery is near room temperature under the null field, and specific inductivity is 10
4The order of magnitude, along with the increase of electric field, Curie temperature is to high-temperature mobile, and specific inductivity descends.
Fig. 3 is barium strontium calcium titanate pyroelectric ceramic material dielectric loss variation with temperature graphic representation under applying direct current electric field that the present embodiment makes, as seen from Figure 3: electric field has reduced ceramic dielectric loss, under the 700V/mm electric field, the dielectric loss at Curie temperature place is lower than 5 ‰.
Fig. 4 is that the barium strontium calcium titanate pyroelectric ceramic material 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 4: electric field so that the pyroelectric coefficient peak to high-temperature mobile, the pyroelectric coefficient peak value increases, under the 500V/mm electric field, the pyroelectric coefficient peak value is maximum, is about 30.36 * 10
-8C/cm
2K.
In addition, the sample that sinters is processed into desired size, ultrasonic cleaning, silk screen printing silver slurry, oven dry is at 650～750 ℃ of lower insulations 20～40 minutes, the dielectric of specimen and pyroelectric property under the 700V/mm direct-current biasing.
Above-mentioned the performance test results is shown in Table 1.
Embodiment 2
The difference of the present embodiment and embodiment 1 only is: according to general formula (Ba
0.6Sr
0.3Ca
0.1)
0.991Y
0.009Ti
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder.
All the other contents of the present embodiment are identical with described in the embodiment 1 all, and the performance test results of obtained sample is shown in Table 1.
The difference of the present embodiment and embodiment 1 only is: according to general formula (Ba
0.6Sr
0.3Ca
0.1)
0.995Y
0.005Ti
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder.
All the other contents of the present embodiment are identical with described in the embodiment 1 all, and the performance test results of obtained sample is shown in Table 1.
Embodiment 4
The difference of the present embodiment and embodiment 1 only is: according to general formula (Ba
0.6Sr
0.3Ca
0.1)
0.997Y
0.003Ti
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder.
All the other contents of the present embodiment are identical with described in the embodiment 1 all, and the performance test results of obtained sample is shown in Table 1.
Embodiment 5
The difference of the present embodiment and embodiment 1 only is: according to general formula (Ba
0.6Sr
0.3Ca
0.1)
0.999Y
0.001Ti
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder.
All the other contents of the present embodiment are identical with described in the embodiment 1 all, and the performance test results of obtained sample is shown in Table 1.
Table 1 embodiment 1～5 obtained sample the performance test results under the 700V/mm electric field
By as seen from Table 1: the barium strontium calcium titanate pyroelectric ceramic material through Y, Mn doping vario-property of the present invention not only has grain-size little (1～3 micron), specific inductivity large (10
4The order of magnitude), and have higher pyroelectric property, when the 700V/mm bias field, its pyroelectric coefficient can reach (25～35) * 10
-8C/cm
2K surveys the figure of merit and can reach (7～9) * 10
-5Pa
-1/2, can satisfy and make the requirement of non-refrigerating infrared focal plane performance of devices, effectively solved the contradiction between fine grain size and the high pyroelectric property.
Should be noted that at last, above embodiment is unrestricted the present invention in order to technical scheme of the present invention to be described only, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (9)
1. preparation method through the barium strontium calcium titanate pyroelectric ceramic material of doping vario-property, described pyroelectric ceramic material has following composition general formula: (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3, x=0.001 ~ 0.010 wherein; It is characterized in that, comprise following concrete steps:
A) at first according to general formula (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Take by weighing the BaCO of stoichiometric ratio
3, SrCO
3, CaCO
3, TiO
2, Y
2O
3And MnCO
3Each powder mixes all powders with wet ball grinding technique;
B) briquetting after the oven dry, synthetic under air atmosphere, synthesis temperature is 1000 ~ 1200 ℃, soaking time is 1 ~ 3 hour, is consisted of (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder;
C) with step b) obtain consist of (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder pulverize, sieve, with wet ball grinding technique powder is mixed again;
D) oven dry adds binding agent, through granulation, ageing, sieve, moulding, plastic removal step, to make (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Base substrate;
E) with steps d) (the Ba that obtains
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Base substrate carries out sintering under oxygen atmosphere, the processing condition of sintering are: the speed with 1 ~ 4 ℃/min heats up; Begin logical oxygen when being warmed up to 800 ~ 1000 ℃, oxygen flow is 1 ~ 3L/min; When being warmed up to 1400 ~ 1450 ℃, be incubated 1 ~ 2 hour; Cool to room temperature with the furnace, close oxygen.
2. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1, it is characterized in that, the wet ball grinding processing condition of step in a) are: the mass ratio of ball milling material and ball-milling medium and deionized water is 1:(1.0 ~ 2.0): (1.0 ~ 1.5), Ball-milling Time is 12 ~ 24 hours, and described ball-milling medium is steel ball, zirconium ball or agate ball.
3. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that step b) in: the deionized water that after oven dry, before the briquetting, adds total powder 10% quality.
4. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that step c) in: (Ba
0.6Sr
0.3Ca
0.1)
1-xY
xTi
0.999Mn
0.001O
3Powder is crossed 40 mesh sieves before carrying out wet ball grinding.
5. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1, it is characterized in that, step c) the wet ball grinding processing condition in are: the mass ratio of ball milling 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, and described ball-milling medium is steel ball, zirconium ball or agate ball.
6. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that steps d) described in binding agent be polyvinyl alcohol (PVA), add-on is 3 ~ 6% of powder quality.
7. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that steps d) in digestion time be 22 ~ 26 hours.
8. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that steps d) in: 20 mesh sieves before moulding, crossed.
9. the preparation method of the barium strontium calcium titanate pyroelectric ceramic material through doping vario-property according to claim 1 is characterized in that steps d) in: the temperature of plastic removal is 750 ~ 850 ℃.
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| CN103011803A (en) * | 2012-12-11 | 2013-04-03 | 浙江大学 | Leadless ceramic with high thermoelectric effect and preparation method thereof |
| CN104098332A (en) * | 2013-04-15 | 2014-10-15 | 中国科学院上海硅酸盐研究所 | Leadless pyroelectric ceramic material and preparation method thereof |
| CN103265288B (en) * | 2013-05-10 | 2015-10-14 | 伊犁师范学院 | Large dielectric constant piezoelectric ceramic and preparation method thereof |
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| CN1546426A (en) * | 2003-12-08 | 2004-11-17 | 华中科技大学 | Barium strontium titanate ferroelectric film material and its preparation method |
| CN101625268A (en) * | 2009-07-07 | 2010-01-13 | 华中科技大学 | Preparation method of porous field pyroelectric ceramic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546426A (en) * | 2003-12-08 | 2004-11-17 | 华中科技大学 | Barium strontium titanate ferroelectric film material and its preparation method |
| CN101625268A (en) * | 2009-07-07 | 2010-01-13 | 华中科技大学 | Preparation method of porous field pyroelectric ceramic material |
Non-Patent Citations (2)
| Title |
|---|
| Dae-Seok Kang et al..Dielectric and pyroelectric properties of barium strontium calcium titanate ceramics.《Journal of the European Ceramic Society》.2003,第23卷第515-518页. * |
| Sung-Soo Lim et al..Dielectric and pyroelectric properties of (Ba,Sr,Ca) ceramics for uncooled infrared detectors.《Japanese Journal of Applied Physics》.2000,第39卷第4835-4838页. * |
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