CN104098330A - Method for preparing high-performance BST (barium strontium titanate) pyroelectric ceramics by adopting post-annealing process - Google Patents

Method for preparing high-performance BST (barium strontium titanate) pyroelectric ceramics by adopting post-annealing process Download PDF

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CN104098330A
CN104098330A CN201410350073.3A CN201410350073A CN104098330A CN 104098330 A CN104098330 A CN 104098330A CN 201410350073 A CN201410350073 A CN 201410350073A CN 104098330 A CN104098330 A CN 104098330A
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strontium
bst
barium
annealing
ball
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CN104098330B (en
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毛朝梁
姚春华
曹菲
陈建和
王根水
董显林
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relate to a method for preparing high-performance BST (barium strontium titanate) pyroelectric ceramics by adopting a post-annealing process. According to the method, BST ceramics obtained through sintering is subjected to annealing at the oxygen atmosphere, the annealing temperature ranges from 800 DEG C to 1,250 DEG C, the annealing time ranges from 2 hours to 5 hours, and then the high-performance BST pyroelectric ceramics can be prepared. According to the method for preparing the high-performance BST pyroelectric ceramics by adopting the post-annealing process, the annealing treatment is performed after the BST pyroelectric ceramics is obtained through sintering, and the high-performance BST pyroelectric ceramics can be prepared; the dielectric constant is high and can be higher than 9,500; the pyroelectric coefficient is high and can be higher than 18*10<-8>C/cm<2>K; and further, a sample is high in purity and performance and good in uniformity, manufacturing requirements of an uncooled infrared focal plane device can be met, and the problem that the BST ceramics cannot be sintered to high density is effectively solved.

Description

Adopt post growth annealing to prepare the method for high-performance strontium-barium titanate pyroelectric ceramics
Technical field
The present invention relates to a kind of method that adopts post growth annealing to prepare high-performance BST pyroelectric ceramics, belong to pyroelectric ceramic material technical field.
Background technology
Strontium-barium titanate (Ba xsr 1-xtiO 3(0<x<1), BST) Curie temperature is adjustable, dielectric loss is low, process the features such as easy owing to having for stupalith, becomes important candidate material for thermoelectric type non-refrigerating infrared focal plane.
BST pyroelectric ceramics is in the time being made into non-refrigerating infrared focal plane device, what adopt is novel dielectric operating mode, be operated near Curie temperature (Curie temperature is in room temperature), and apply certain direct current biasing electric field, can utilize like this its intrinsic pyroelectric effect and field to cause pyroelectric effect (velocity of variation of dielectric constant with temperature), formula (1) has shown its pyroelectric coefficient simultaneously:
p ( T ) = ( &PartialD; D &PartialD; T ) E = p 0 ( T ) + &epsiv; 0 &Integral; 0 E &PartialD; &epsiv; &PartialD; T dE - - - ( 1 )
In formula, p is pyroelectric coefficient, and D is electricdisplacement, p 0for intrinsic pyroelectric coefficient, E is added electric field, and T is temperature, ε 0for permittivity of vacuum, ε is relative permittivity.From formula, can find out, the specific inductivity of pottery is higher, and pyroelectric coefficient is larger, is more conducive to its application.Therefore, high-k, high pyroelectric coefficient are extremely important to the practical application of BST pyroelectric ceramics.
But, generally, the BST pottery that adopts ordinary process to prepare, its specific inductivity is not high, pyroelectric coefficient is also on the low side.Therefore, how effectively improving specific inductivity and the pyroelectric coefficient of BST pottery, make BST pottery 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
The problem that is difficult to prepare high-performance BST pyroelectric ceramics for solving prior art, the invention provides a kind of method that adopts post growth annealing to prepare high-performance BST pyroelectric ceramics, to meet the requirement of current non-refrigerating infrared focal plane device to BST material.
At this, the invention provides a kind of method that adopts post growth annealing to prepare high-performance strontium-barium titanate pyroelectric ceramics, the barium-strontium titanate ceramic obtaining through sintering is annealed under oxygen atmosphere, annealing temperature is 800～1250 DEG C, annealing time is 2～5 hours, can make high-performance strontium-barium titanate pyroelectric ceramics.
The present invention carries out after annealing processing by after making barium-strontium titanate ceramic at sintering to it, can make high performance strontium-barium titanate pyroelectric ceramics, and its specific inductivity is high, can reach more than 9500, and pyroelectric coefficient is high, can reach 18 × 10 - 8c/cm 2more than K, and sample purity is high, performance is high, good uniformity, can meet the requirement of making non-refrigerating infrared focal plane device, has effectively solved the problem that BST pottery is difficult to sinter to high-compactness.
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 described annealing, the speed of 1～4 DEG C/min rises to described annealing temperature.
Preferably, in described annealing, the flow that passes into oxygen is 1～3L/ minute.
The null field relative permittivity peak value >9800 of the prepared high-performance strontium-barium titanate of the present invention pyroelectric ceramics, pyroelectric coefficient peak value >18 × 10 -8c/cm 2k.
Preferably, described the barium-strontium titanate ceramic obtaining through sintering is made by following steps:
A) take the BaCO of stoichiometric ratio according to the chemical formula of high-performance strontium-barium titanate pyroelectric ceramics to be prepared 3, SrCO 3, TiO 2the oxide compound of powder and doped element and/or carbonate powder, mix all powders by wet ball grinding technique and obtain raw mixture;
B) raw mixture of gained is dried to rear briquetting, synthetic in air, synthesis temperature is 1000～1200 DEG C, and soaking time is 1～3 hour, obtains strontium-barium titanate piece;
C) strontium-barium titanate piece step b) being obtained is pulverized, is sieved, make powder refining by wet ball grinding technique, discharging post-drying, adds the binding agent of specified amount, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal, make strontium-barium titanate base substrate;
D) strontium-barium titanate base substrate step c) being obtained carries out sintering under oxygen atmosphere, and sintering temperature is 1350～1450 DEG C, and soaking time is 1～5 hour, makes the described barium-strontium titanate ceramic obtaining through sintering.
Wherein, described doped element can comprise at least one in Ca, Y, Mn, Sm and Fe.
Preferably, the wet ball grinding processing condition of step in a) 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, step b) in, after oven dry, before briquetting, add the deionized water of total powder 4%～10% quality.
Preferably, step c) in, barium-strontium titanate powder is carrying out before wet ball grinding crossing 40 mesh sieves.
Preferably, step c) in, described wet ball grinding processing condition are: 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.
Preferably, described binding agent is that mass concentration is 2%～5% polyvinyl alcohol (PVA) solution, and the add-on of polyvinyl alcohol solution is 2%～5% of barium-strontium titanate powder quality.
Preferably, step c) in, digestion time is 22～26 hours.
Preferably, step c) in, plastic removal temperature is 750～850 DEG C.
Preferably, steps d) in, the processing condition of described sintering are: heat up with the speed of 1～4 DEG C/min, start logical oxygen in the time being warming up to 800～1000 DEG C, oxygen flow is 1～3L/ minute; In the time being warming up to 1350～1450 DEG C, be incubated 1～5 hour; Cool to room temperature with the furnace, close oxygen, obtain barium-strontium titanate ceramic.
By method of the present invention, can prepare the BST pyroelectric ceramics that specific inductivity is high, pyroelectric coefficient is high, thereby meet the requirement of current non-refrigerating infrared focal plane device to BST material.
Brief description of the drawings
Fig. 1 is the BST pottery that makes of embodiment 1 and embodiment 2 and the change curve comparison diagram of unannealed sample (comparative example 1) dielectric constant with temperature under applying direct current electric field;
Fig. 2 is the ceramic pyroelectric coefficient variation with temperature curve comparison figure that adopts Quasi-static Method to test under applying direct current electric field with unannealed sample (comparative example 1) of BST that embodiment 1 and embodiment 2 make.
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.
The present invention adopts post growth annealing to prepare high-performance strontium-barium titanate (BST) pyroelectric ceramics.After annealing atmosphere can be oxygen, and annealing temperature can be 800～1250 DEG C, and annealing time can be 2～5 hours.
In after annealing, can rise to described annealing temperature with the speed of 1～4 DEG C/min.In addition, in after annealing, the flow that passes into oxygen can be 1～3L/ minute.
The material that carries out after annealing processing can be the barium-strontium titanate ceramic obtaining through sintering.Before after annealing is processed, can also be by barium-strontium titanate ceramic through techniques such as cutting, grinding and polishings, be processed into the size needing.
In one example, the processing condition of described after annealing processing are: heat up with the speed of 1～4 DEG C/min, and pass into oxygen, oxygen flow is 1～3L/ minute; While being warming up to 800～1250 DEG C, be incubated 2～5 hours; Cool to room temperature with the furnace, close oxygen, can make high-performance BST pottery.
Fig. 1 illustrates the change curve comparison diagram of BST pottery that the present invention makes and unannealed sample dielectric constant with temperature under applying direct current electric field, and Fig. 2 illustrates that BST pottery that the present invention makes and unannealed sample adopt the pyroelectric coefficient variation with temperature curve comparison figure of Quasi-static Method test under applying direct current electric field.As seen from Figure 1, Figure 2, the BST pyroelectric ceramics that adopts the present invention to prepare has specific inductivity high (relative permittivity >9800), high (pyroelectric coefficient >18 × 10 under 850V/mm of pyroelectric coefficient -8ccm -2k -1) advantage, the sample of annealing at two temperature can improve respectively 22% and 38%, 13% and 25% than unannealed sample specific inductivity, pyroelectric coefficient, increasing degree is very large, is conducive to very much its application at non-refrigerating infrared focal plane.
Should be understood that the strontium-barium titanate described in the present invention (BST) pyroelectric ceramics composition do not limit, for example, can be unadulterated strontium-barium titanate (Ba xsr 1-xtiO 3(0<x<1), BST), can be also the strontium-barium titanate of doping, wherein doped element includes but not limited at least one in Ca, Y, Mn, Sm and Fe.
The preparation method of the described barium-strontium titanate ceramic obtaining through sintering does not limit, for example, can make with the following method:
A) first according to Formula B a xsr 1-xtiO 3take the BaCO of stoichiometric ratio 3, SrCO 3and TiO 2powder, mixes all powders by wet ball grinding technique, in general formula, can add doped element, and as Ca, Y, Mn, Sm, Fe etc., doped element for example can add with the form of oxide compound and/or carbonate;
B) dry rear briquetting, synthetic in air, synthesis temperature is 1000～1200 DEG C, and soaking time is 1～3 hour, obtains BST piece;
C) BST piece step b) being obtained is pulverized, is sieved, and makes powder refining by wet ball grinding technique;
D) discharging post-drying, adds a certain amount of binding agent, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal, make BST idiosome;
E) by steps d) the BST base substrate that obtains carries out sintering under oxygen atmosphere, and sintering process conditions is: heat up with the speed of 1～4 DEG C/min, start logical oxygen in the time being warming up to 800～1000 DEG C, oxygen flow is 1～3L/ minute; In the time being warming up to 1350～1450 DEG C, be incubated 1～5 hour; Cool to room temperature with the furnace, close oxygen, obtain BST pottery.
The wet ball grinding processing condition of step in a) 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 b) in, can be after oven dry, add the deionized water of total powder 4%～10% quality before briquetting.
Step c) in, BST powder is carrying out can crossing 40 mesh sieves before wet ball grinding.
The wet ball grinding processing condition of step in c) are carved and are: 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.
Steps d) described in binding agent can be for example that mass concentration is 2%～5% polyvinyl alcohol (PVA) solution, the add-on of PVA solution is 2%～5% of BST powder quality.
Steps d) in digestion time can be 22～26 hours.
Steps d) in plastic removal temperature can be 750～850 DEG C.
The present invention compared with prior art, has following beneficial effect:
1) BST pyroelectric ceramics specific inductivity of the present invention is high, can reach more than 9500, and pyroelectric coefficient is high, can reach 18 × 10 -8c/cm 2more than K, and sample purity is high, performance is high, good uniformity, can meet the requirement of making non-refrigerating infrared focal plane device, has 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 specific 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 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
First take BaCO 3, SrCO 3and TiO 2powder, and add a small amount of CaCO 3, Y 2o 3, 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 DEG C, soaking time is 2 hours, obtains BST piece; Pulverize, cross 40 mesh sieves, then add the ZnO powder of 2.7wt%, powder is mixed by wet ball grinding technique; 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 DEG C of plastic removals, makes BST base substrate; By BST base substrate sintering under oxygen, the condition of sintering is: heat up with the speed of 2.0 DEG C/min; In the time being warming up to 800 DEG C, start logical oxygen, oxygen flow is 2L/ minute; In the time being warming up to 1350 DEG C, be incubated 5 hours; Be cooled to room temperature, close oxygen.
The sample sintering, through techniques such as cutting, grinding and polishings, is processed into the size needing, then under oxygen atmosphere, anneals, annealing process condition is: heat up with the speed of 1～4 DEG C/min, and pass into oxygen, oxygen flow is 1～3L/ minute; While being warming up to 800 DEG C, be incubated 2 hours; Cool to room temperature with the furnace, close oxygen.
The sample of having annealed is processed into the size needing, ultrasonic cleaning, silk screen printing silver slurry, dries, and at 700 DEG C, is incubated 30 minutes, tests dielectric and the pyroelectric property of sample under direct current (DC) bias.
Embodiment 2
The annealing temperature of BST pottery is 1250 DEG C, and annealing time is 2 hours, and all the other contents are with described in embodiment 1.
Comparative example 1
Described in embodiment 1, obtain the sample sintering, and do not carry out after annealing processing.
Fig. 1 is the change curve comparison diagram of unannealed sample dielectric constant with temperature under applying direct current electric field of making of the BST pyroelectric ceramics that makes of embodiment 1, embodiment 2 and comparative example 1, as seen from Figure 1: the Curie temperature of sample is all near room temperature, specific inductivity peak value under 800 DEG C, 1250 DEG C annealing specimen null fields is respectively 9851 and 11119, unannealed sample is 8085, improve respectively 22% and 38%, increasing degree is very large, and this is very beneficial for the raising of its pyroelectric coefficient.
Fig. 2 is that the unannealed sample that the BST pyroelectric ceramics that makes of embodiment 1, embodiment 2 and comparative example 1 make adopts the pyroelectric coefficient of Quasi-static Method test with the change curve comparison diagram of temperature and applying direct current electric field, as seen from Figure 2: 800 DEG C, 1250 DEG C annealing specimens are under 850V/mm electric field, and pyroelectric coefficient peak value is respectively 18.8 × 10 -8ccm -2k -1with 20.9 × 10 -8ccm -2k -1, unannealed sample is 16.7 × 10 -8ccm -2k -1, improving respectively 13% and 25%, increasing degree is very large, and this will be conducive to it and be applied to non-refrigerating infrared focal plane.
In sum, the BST pyroelectric ceramics that adopts the present invention to prepare has specific inductivity high (relative permittivity >9800), high (pyroelectric coefficient >18 × 10 under 850V/mm of pyroelectric coefficient -8ccm -2k -1) advantage, the sample of annealing at two temperature can improve respectively 22% and 38%, 13% and 25% than unannealed sample specific inductivity, pyroelectric coefficient, increasing degree is very large, is conducive to very much its application at non-refrigerating infrared focal plane.
The present invention efficiently solves the difficult problem that general technology is difficult to prepare high-k and high pyroelectric coefficient BST pottery, 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 (10)

1. a method that adopts post growth annealing to prepare high-performance strontium-barium titanate pyroelectric ceramics, it is characterized in that, the barium-strontium titanate ceramic obtaining through sintering is annealed under oxygen atmosphere, annealing temperature is 800～1250 DEG C, annealing time is 2～5 hours, can make high-performance strontium-barium titanate pyroelectric ceramics.
2. method according to claim 1, is characterized in that, in described after annealing, rises to described annealing temperature with the speed of 1～4 DEG C/min.
3. method according to claim 1 and 2, is characterized in that, in described after annealing, the flow that passes into oxygen is 1～3L/ minute.
4. according to the method in any one of claims 1 to 3, it is characterized in that the null field relative permittivity peak value >9800 of prepared high-performance strontium-barium titanate pyroelectric ceramics, pyroelectric coefficient peak value >18 × 10 -8c/cm 2k.
5. according to the method described in any one in claim 1 to 4, it is characterized in that, described the barium-strontium titanate ceramic obtaining through sintering made by following steps:
A) take the BaCO of stoichiometric ratio according to the chemical formula of high-performance strontium-barium titanate pyroelectric ceramics to be prepared 3, SrCO 3, TiO 2the oxide compound of powder and doped element and/or carbonate powder, mix all powders by wet ball grinding technique and obtain raw mixture;
B) raw mixture of gained is dried to rear briquetting, synthetic in air, synthesis temperature is 1000～1200 DEG C, and soaking time is 1～3 hour, obtains strontium-barium titanate piece;
C) strontium-barium titanate piece step b) being obtained is pulverized, is sieved, make powder refining by wet ball grinding technique, discharging post-drying, adds the binding agent of specified amount, through granulation, ageing, sieve after precompressed again, isostatic pressing, plastic removal, make strontium-barium titanate base substrate;
D) strontium-barium titanate base substrate step c) being obtained carries out sintering under oxygen atmosphere, and sintering temperature is 1350～1450 DEG C, and soaking time is 1～5 hour, makes the described barium-strontium titanate ceramic obtaining through sintering.
6. method according to claim 5, it is characterized in that, the wet ball grinding processing condition of step in a) 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, and described ball-milling medium is agate ball.
7. according to the method described in claim 5 or 6, it is characterized in that, step b) in, after oven dry, before briquetting, add the deionized water of total powder 4%～10% quality.
8. according to the method described in any one in claim 5 to 7, it is characterized in that, step c) in,
Barium-strontium titanate powder is carrying out before wet ball grinding crossing 40 mesh sieves;
Described wet ball grinding processing condition are: 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;
Described binding agent is that mass concentration is 2%～5% polyvinyl alcohol solution, and the add-on of polyvinyl alcohol solution is 2%～5% of barium-strontium titanate powder quality.
9. according to the method described in any one in claim 5 to 8, it is characterized in that, step c) in,
Digestion time is 22～26 hours;
Plastic removal temperature is 750～850 DEG C.
10. according to the method described in any one in claim 5 to 9, it is characterized in that steps d) in, the processing condition of described sintering are: the speed with 1～4 DEG C/min heats up, in the time being warming up to 800～1000 DEG C, start logical oxygen, oxygen flow is 1～3L/min; In the time being warming up to 1350～1450 DEG C, be incubated 1～5 hour; Cool to room temperature with the furnace, close oxygen, obtain barium-strontium titanate ceramic.
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CN106116567A (en) * 2016-06-22 2016-11-16 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN114940616A (en) * 2022-04-08 2022-08-26 桂林理工大学 Rare earth modified strontium titanate giant dielectric ceramic material and preparation method thereof
CN115636666A (en) * 2022-12-23 2023-01-24 北京大学口腔医学院 Temperature change antibacterial composition, preparation method and application
CN116041059A (en) * 2023-02-08 2023-05-02 西北工业大学 Preparation method of strontium titanate-based giant dielectric ceramic

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Publication number Priority date Publication date Assignee Title
CN106116567A (en) * 2016-06-22 2016-11-16 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN106116567B (en) * 2016-06-22 2018-11-02 刘和来 The preparation method of high density nano barium titanate titanate ceramics
CN114940616A (en) * 2022-04-08 2022-08-26 桂林理工大学 Rare earth modified strontium titanate giant dielectric ceramic material and preparation method thereof
CN115636666A (en) * 2022-12-23 2023-01-24 北京大学口腔医学院 Temperature change antibacterial composition, preparation method and application
CN116041059A (en) * 2023-02-08 2023-05-02 西北工业大学 Preparation method of strontium titanate-based giant dielectric ceramic
CN116041059B (en) * 2023-02-08 2024-04-02 西北工业大学 Preparation method of strontium titanate-based giant dielectric ceramic

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