CN104557038A - Composite pyroelectric ceramic material and preparation method thereof - Google Patents

Composite pyroelectric ceramic material and preparation method thereof Download PDF

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CN104557038A
CN104557038A CN201410843289.3A CN201410843289A CN104557038A CN 104557038 A CN104557038 A CN 104557038A CN 201410843289 A CN201410843289 A CN 201410843289A CN 104557038 A CN104557038 A CN 104557038A
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CN104557038B (en
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郭栋
王云丽
蔡锴
史丹丹
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Institute of Acoustics CAS
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Abstract

The invention discloses a composite pyroelectric ceramic material and a preparation method thereof. The chemical general formula of the material is Pb {[(Me1/3Nb2/3)x(W1/3Fe2/3)1-x]y(Zr0.9Ti0.1) (1-y) }O3-nMe', wherein Me is Mg or Zn; x and y represent a mole fraction respectively, x is larger than or equal to 0.125 and smaller than or equal to 0.875, and y is larger than or equal to 0.08 and smaller than or equal to 0.11; Me' is a modified element and is one or more of Li, La and Sb, and the molar ratio range n is larger than or equal to 0 mol% and smaller than or equal to 5 mol%. The composite pyroelectric ceramic material has a higher pyroelectric coefficient and adjustable dielectric property, thereby having a better application prospect in various pyroelectric detectors.

Description

A kind of compound system pyroelectric ceramic material and preparation method thereof
Technical field
The present invention relates to field of material technology, particularly relate to a kind of novel four-element complex system pyroelectric ceramic material and preparation method thereof.
Background technology
Pyroelectricity material can be used for infrared eye, infrared thermometer and video camera etc., these equipment obtain a wide range of applications in fields such as flame detecting, environmental pollution monitoring, non-contact type temperature measurement, medical diagnosis, commercial run automatic monitoring, Security alerts.
Current use more widely pyroelectric ceramics is rich zirconium type Pb-based lanthanumdoped zirconate titanates (PZT).But this material at low temperature ferroelectric water chestnut side phase (F rL) to high temperature ferroelectric water chestnut side phase (F rH) first-order phase transition temperature range narrow (2 ~ 3 DEG C), this is unfavorable for its application in infrared acquisition.In PZT, add the stupalith with different transformation temperature make compound system, this F of easily extensible rL-F rHtransition temperature range is a kind of effective way improving its pyroelectricity material performance.Lead iron tungstate Pb (W 1/3fe 2/3) O 3(PFW) be a kind of ferroelectric material of complex perovskite structure, have typical Relaxation Ferroelectrics characteristic, its specific inductivity is larger, phase transition temperature range is wide, and there is lower sintering temperature (Current AppliedPhysics 2011, Vol 11, S154-S156).What effect was similar therewith also has Pb (Mg 1/3nb 2/3) O 3and Pb (Zn (PMN) 1/3nb 2/3) O 3(PZN), these systems and PZT can form continuous solid solution.Therefore a small amount of the graduates of three governmental examinations quaternary system and rich zirconium type binary PZT compound is utilized can to prepare the polynary system pyroelectricity material of modification, and these materials can obtain regulatable comprehensive electrical performance in certain limit by the adjustment of different components, thus the different composite requests of different pyroelectric electric device to performance can be met.In addition, form suitable multivariate solid solution system and also can obtain fine and close pottery in wider sintering range.
But, there is higher thermal at present and release electrostrictive coefficient and the adjustable novel quaternary composite structure pyroelectric ceramics system of electrical property is but very limited.
Summary of the invention
Embodiments provide a kind of compound system pyroelectric ceramic material and preparation method thereof.Compound system pyroelectric ceramic material provided by the invention, has higher pyroelectric coefficient and adjustable dielectric properties, thus in various pyroelectric detector, has better application prospect.
First aspect, embodiments provides a kind of compound system pyroelectric ceramic material and preparation method thereof, and the chemical general formula of described material is:
Pb{[(Me 1/3Nb 2/3) x(W 1/3Fe 2/3) 1-x] y(Zr 0.9Ti 0.1) 1-y}O 3-nMe’；
Wherein, Me is the one in Mg or Zn; X, y represent molar fraction respectively, 0.125≤x≤0.875,0.08≤y≤0.11; Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.
Second aspect, embodiments provide a kind of preparation method of the pyroelectric ceramic material as described in above-mentioned first aspect, described preparation method comprises:
By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder, and by MgO and Nb 2o 5or ZnO and Nb 2o 5wherein one group press 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6or ZnNb 2o 6presoma powder;
By Pb 3o 4, ZrO 2, TiO 2, FeWO 4presoma powder, MnNb 2o 6or ZnNb 2o 6the oxide compound of presoma powder, modifying element Me ' or salt are according to the molar ratio weighing of the chemical general formula described in the claims 1, and then mixing and ball milling, obtains slurry;
Described slurry is dried, sieve after carry out pre-burning, and the block ball milling again described pre-burning obtained;
The slurry obtained after ball milling is again dried and obtains powder, in described powder, add polyvinyl alcohol (PVA) binding agent carry out grinding granulation, sieve after ageing placement, obtain powder;
Described powder pressing is become ceramic body;
Described ceramic blank-body exhaust glue is placed in close crucible, sinters ceramic body into;
Described ceramic body is polished, polishing, after painting silver electrode, puts into oil bath and heat up, apply voltage and polarize, after cooling, namely obtain described pyroelectric ceramic material.
Preferably, described calcined temperature is 750 DEG C ~ 900 DEG C, and the time is 1.5 ~ 5 hours.
Preferably, described PVA caking agent is specially: the PVA aqueous solution of 1wt% ~ 6wt%.
Preferably, the time of described ageing is no more than 12 hours.
Preferably, the temperature of described sintering is 1000 DEG C ~ 1200 DEG C, and the time is 2 ~ 5 hours.
Preferably, the temperature of described polarization is 80 DEG C ~ 120 DEG C, and the strength of electric field of polarization is 3kV/mm ~ 5kV/mm, and the time of polarization is 10 ~ 20 minutes.
Novel four-element complex system pyroelectric ceramic material the Pb{ [(Me that the embodiment of the present invention provides 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3-nMe ' has higher pyroelectric coefficient (λ=5 × 10 -8ccm -2k -1~ 20 × 10 -8ccm -2k -1), suitable DIELECTRIC CONSTANT ε r(100 ~ 800) and lower dielectric loss tan δ (0.008 ~ 0.030), and these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be obtained at a relatively low sintering temperature, thus this material and its preparation method can be applicable to different pyroelectric detect devices.
Accompanying drawing explanation
Below by drawings and Examples, the technical scheme of the embodiment of the present invention is described in further detail.
Preparation method's schema of the compound system pyroelectric ceramic material that Fig. 1 provides for the embodiment of the present invention 2;
The preparation method that Fig. 2 provides for the embodiment of the present invention 3 sinters at 1100 DEG C, be incubated 2.5 hours after gained four-element complex system pyroelectric ceramic material Pb{ [(Mg 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3scanning electron microscope (SEM) image;
The preparation method that Fig. 3 provides for the embodiment of the present invention 3 sinters at 1100 DEG C, be incubated 2.5 hours after gained four-element complex system pyroelectric ceramic material Pb{ [(Mg 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3pyroelectricity curve;
The preparation method that Fig. 4 provides for the embodiment of the present invention 5 sinters at 1120 DEG C, be incubated 3 hours after gained four-element complex system pyroelectric ceramic material Pb{ [(Zn 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3scanning electron microscope (SEM) image;
The preparation method that Fig. 5 provides for the embodiment of the present invention 5 sinters at 1120 DEG C, be incubated 3 hours after gained compound system pyroelectric ceramic material Pb{ [(Zn 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3pyroelectricity curve.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but is not intended to limit the scope of the invention.
Embodiment 1
The embodiment of the present invention 1 provides a kind of novel four-element complex system pyroelectric ceramic material, and its chemical general formula is: Pb{ [(Me 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3-nMe ';
Wherein, Me is the one in Mg or Zn; X, y represent molar fraction respectively, 0.125≤x≤0.875,0.08≤y≤0.11; The conventional modifying element of Me ' for mixing, can be one or more in Li, La or Sb, its molar ratio range be 0mol%≤n≤5mol%.
Novel four-element complex system pyroelectric ceramic material the Pb{ [(Me that the embodiment of the present invention provides 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3-nMe ' has higher pyroelectric coefficient (λ=5 × 10 -8ccm -2k -1~ 20 × 10 -8ccm -2k -1), suitable specific inductivity (100 ~ 800) and lower dielectric loss (0.008 ~ 0.030), and these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be obtained at a relatively low sintering temperature, thus this material can be applicable to different pyroelectric detect devices.
Embodiment 2
Present embodiments provide the preparation method of the pyroelectric ceramic material in above-described embodiment 1, as shown in Figure 1, comprising:
Step 201, by Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder, and by MgO and Nb 2o 5or ZnO and Nb 2o 5wherein one group press 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6or ZnNb 2o 6presoma powder;
Step 202, by Pb 3o 4, ZrO 2, TiO 2, FeWO 4presoma powder, MnNb 2o 6or ZnNb 2o 6the oxide compound of presoma powder, modifying element Me ' or salt are according to chemical general formula Pb{ [(Me 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3the molar ratio weighing of-nMe ', then mixing and ball milling, obtain slurry;
Wherein, Me is the one in Mg or Zn; X, y represent molar fraction respectively, 0.125≤x≤0.875,0.08≤y≤0.11; Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.
Step 203, described slurry is dried, sieve after carry out pre-burning, and the block ball milling again described pre-burning obtained;
Concrete, described calcined temperature is 750 DEG C ~ 900 DEG C, and the time is 1.5 ~ 5 hours.
Step 204, dries the slurry obtained after ball milling again and obtains powder, add polyvinyl alcohol (PVA) binding agent and carry out grinding granulation in described powder, sieves, obtain powder after ageing placement;
Concrete, described PVA caking agent is specially: the PVA aqueous solution of 1wt% ~ 6wt%, and the time of described ageing is no more than 12 hours.
Step 205, becomes ceramic body by described powder pressing;
Step 206, is placed in close crucible by described ceramic blank-body exhaust glue, sinters ceramic body into;
Concrete, sintering temperature can be preferably 1000 DEG C ~ 1200 DEG C, and the time of sintering is preferably 2 ~ 5 hours.
Step 207, polishes to described ceramic body, polishing, after painting silver electrode, puts into oil bath and heat up, apply voltage and polarize, namely obtain described pyroelectric ceramic material after cooling.
Concrete, polarization process comprises:
In the silicone oil of 80 DEG C ~ 120 DEG C, described ceramic body is polarized 10 ~ 20 minutes under the polarized electric field intensity of 3kV/mm ~ 5kV/mm.
The preparation method of the novel four-element complex system pyroelectric ceramic material that the present embodiment provides, can be used in the compound system pyroelectric ceramic material prepared described in above-described embodiment 1.The material prepared has higher pyroelectric coefficient (λ=5 × 10 -8ccm -2k -1~ 20 × 10 -8ccm -2k -1), suitable specific inductivity (100 ~ 800) and lower dielectric loss (0.008 ~ 0.030), and these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be obtained at a relatively low sintering temperature, thus this material and its preparation method can be applicable to different pyroelectric detect devices.
The technical scheme provided for a better understanding of the present invention, the following detailed process preparing compound system pyroelectric ceramic material with multiple specific examples preparation method that application the above embodiment of the present invention provides respectively, and performance.
Embodiment 3
By MgO and Nb 2o 5by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6presoma powder; By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder.By Pb 3o 4, ZrO 2, TiO 2, MgNb 2o 6presoma powder and FeWO 4pb{ [(Mg pressed by presoma powder 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 750 DEG C of pre-burnings 2 hours.The block obtained after pre-burning is carried out ball milling, oven dry again, and adds 5%PVA granulation, ageing 6 hours, being pressed into diameter after sieving is 15mm, and thickness is the base substrate of about 1.5mm, sinters 2.5 hours, obtain ceramic body after binder removal at 1100 DEG C.By gained ceramic body through polishing, polishing, by silver after, with 4kV/mm electric field polarization 20 minutes in 120 DEG C of silicone oil, obtained required compound system pyroelectric ceramic material Pb{ [(Mg after cooling 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3ceramics sample.
Test gained comprehensive electrochemical properties is: λ is 5 × 10 -8ccm -2k -1~ 14 × 10 -8ccm -2k -1, ε r=561, tan δ=0.008.Scanning electron microscope (SEM) image is shown in Fig. 2, and pyroelectricity curve is shown in Fig. 3.
Embodiment 4
By MgO and Nb 2o 5by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6presoma powder; By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder.By Pb 3o 4, ZrO 2, TiO 2, MgNb 2o 6presoma powder and FeWO 4pb{ [(Mg pressed by presoma powder 1/3nb 2/3) 0.875(W 1/3fe 2/3) 0.125] 0.09(Zr 0.9ti 0.1) 0.91o 3molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 750 DEG C of pre-burnings 2 hours.The block obtained after pre-burning is carried out ball milling, oven dry again, and adds 6%PVA granulation, ageing 6 hours, being pressed into diameter after sieving is 15mm, and thickness is the base substrate of about 1.5mm, sinters 3 hours, obtain ceramic body after binder removal at 1100 DEG C.By gained ceramic body through polishing, polishing, by silver after, with 4kV/mm electric field polarization 10 minutes in 110 DEG C of silicone oil, obtained required compound system pyroelectric ceramic material Pb{ [(Mg after cooling 1/3nb 2/3) 0.875(W 1/3fe 2/3) 0.125] 0.09(Zr 0.9ti 0.1) 0.91o 3ceramics sample.
Test gained comprehensive electrochemical properties is: λ is 8 × 10 -8ccm -2k -1~ 11 × 10 -8ccm -2k -1, ε r=313, tan δ=0.017.
Embodiment 5
By ZnO and Nb 2o 5by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making ZnNb 2o 6presoma powder; By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder.By Pb 3o 4, ZrO 2, TiO 2, ZnNb 2o 6presoma powder and FeWO 4pb{ [(Zn pressed by presoma powder 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 800 DEG C of pre-burnings 2 hours.The block obtained after pre-burning is carried out ball milling, oven dry again, and adds 5%PVA granulation, ageing 6 hours, being pressed into diameter after sieving is 15mm, and thickness is the base substrate of about 1.5mm, sinters 3 hours, obtain ceramic body after binder removal at 1120 DEG C.By gained ceramic body through polishing, polishing, by silver after, with 4kV/mm electric field polarization 10 minutes in 120 DEG C of silicone oil, obtained required compound system pyroelectric ceramic material Pb{ [(Zn after cooling 1/3nb 2/3) 0.25(W 1/3fe 2/3) 0.75] 0.08(Zr 0.9ti 0.1) 0.92o 3ceramics sample.
Test gained comprehensive electrochemical properties is: λ is 6 × 10 -8ccm -2k -1~ 17 × 10 -8ccm -2k -1, ε r=407, tan δ=0.025.Scanning electron microscope (SEM) image is shown in Fig. 4, and pyroelectricity curve is shown in Fig. 5.
Embodiment 6
By ZnO and Nb 2o 5by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making ZnNb 2o 6presoma powder; By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder.By Pb 3o 4, ZrO 2, TiO 2, ZnNb 2o 6presoma powder and FeWO 4pb{ [(Zn pressed by presoma powder 1/3nb 2/3) 0.75(W 1/3fe 2/3) 0.25] 0.09(Zr 0.9ti 0.1) 0.91o 3molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 800 DEG C of pre-burnings 2 hours.The block obtained after pre-burning is carried out ball milling, oven dry again, and adds 5%PVA granulation, ageing 10 hours, being pressed into diameter after sieving is 12mm, and thickness is the base substrate of about 1.2mm, sinters 2.5 hours, obtain ceramic body after binder removal at 1150 DEG C.By gained ceramic body through polishing, polishing, by silver after, with 4kV/mm electric field polarization 20 minutes in 120 DEG C of silicone oil, obtained required compound system pyroelectric ceramic material Pb{ [(Zn after cooling 1/3nb 2/3) 0.75(W 1/3fe 2/3) 0.25] 0.09(Zr 0.9ti 0.1) 0.91o 3ceramics sample.
Test gained comprehensive electrochemical properties is: λ is 5 × 10 -8ccm -2k -1~ 14 × 10 -8ccm -2k -1, ε r=204, tan δ=0.029.
Embodiment 7
By MgO and Nb 2o 5by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6presoma powder; By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder.By Pb 3o 4, ZrO 2, TiO 2, La 2o 3presoma powder and FeWO 4pb{ [(Mg pressed by presoma powder 1/3nb 2/3) 0.5(W 1/3fe 2/3) 0.5] 0.11(Zr 0.9ti 0.1) 0.89o 3-0.5mol%La molar ratio weighing, adds anhydrous ethanol medium mixing and ball milling, dries after sieving in 750 DEG C of pre-burnings 2 hours.The block obtained after pre-burning is carried out ball milling, oven dry again, and adds 5%PVA granulation, ageing 6 hours, being pressed into diameter after sieving is 15mm, and thickness is the base substrate of about 1.5mm, sinters 3 hours, obtain ceramic body after binder removal at 1050 DEG C.By gained ceramic body through polishing, polishing, by silver after, with 4kV/mm electric field polarization 20 minutes in 90 DEG C of silicone oil, obtained required compound system pyroelectric ceramic material Pb{ [(Mg after cooling 1/3nb 2/3) 0.5(W 1/3fe 2/3) 0.5] 0.11(Zr 0.9ti 0.1) 0.89o 3the ceramics sample of-0.5mol%La.
Test gained comprehensive electrochemical properties is: λ is 10 × 10 -8ccm -2k -1~ 20 × 10 -8ccm -2k -1, ε r=755, tan δ=0.009.
Above embodiment be premised on technical solution of the present invention under, the detailed enforcement material component provided and concrete preparation process, but protection scope of the present invention is not limited to above-described embodiment.
Novel four-element complex system pyroelectric ceramic material the Pb{ [(Me that the embodiment of the present invention provides 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3-nMe ' has higher pyroelectric coefficient (λ=5 × 10 -8ccm -2k -1~ 20 × 10 -8ccm -2k -1), suitable DIELECTRIC CONSTANT ε r(100 ~ 800) and lower dielectric loss tan δ (0.008 ~ 0.030), and these performances are adjustable in relative broad range, and the ceramic body of dense uniform can be obtained at a relatively low sintering temperature, thus this material and its preparation method can be applicable to different pyroelectric detect devices.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (7)

1. a compound system pyroelectric ceramic material, is characterized in that, the chemical general formula of described material is: Pb{ [(Me 1/3nb 2/3) x(W 1/3fe 2/3) 1-x] y(Zr 0.9ti 0.1) 1-yo 3-nMe ';
Wherein, Me is the one in Mg or Zn; X, y represent molar fraction respectively, 0.125≤x≤0.875,0.08≤y≤0.11; Me ' is modifying element, is one or more in Li, La or Sb, and its molar ratio range is 0mol%≤n≤5mol%.
2., as a preparation method for above-mentioned pyroelectric ceramic material according to claim 1, it is characterized in that, described preparation method comprises:
By Fe 2o 3and WO 3by 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making FeWO 4presoma powder, and by MgO and Nb 2o 5or ZnO and Nb 2o 5wherein one group press 1:1 mixed in molar ratio ball milling, calcine again after drying and grind, making MgNb 2o 6or ZnNb 2o 6presoma powder;
By Pb 3o 4, ZrO 2, TiO 2, FeWO 4presoma powder, MnNb 2o 6or ZnNb 2o 6the oxide compound of presoma powder, modifying element Me ' or salt are according to the molar ratio weighing of the chemical general formula described in the claims 1, and then mixing and ball milling, obtains slurry;
Described slurry is dried, sieve after carry out pre-burning, and the block ball milling again described pre-burning obtained;
The slurry obtained after ball milling is again dried and obtains powder, in described powder, add polyvinyl alcohol (PVA) binding agent carry out grinding granulation, sieve after ageing placement, obtain powder;
Described powder pressing is become ceramic body;
Described ceramic blank-body exhaust glue is placed in close crucible, sinters ceramic body into;
Described ceramic body is polished, polishing, after painting silver electrode, puts into oil bath and heat up, apply voltage and polarize, after cooling, namely obtain described pyroelectric ceramic material.
3. preparation method according to claim 2, is characterized in that, described calcined temperature is 750 DEG C ~ 900 DEG C, and the time is 1.5 ~ 5 hours.
4. preparation method according to claim 2, is characterized in that, described PVA caking agent is specially: the PVA aqueous solution of 1wt% ~ 6wt%.
5. preparation method according to claim 2, is characterized in that, the time of described ageing is no more than 12 hours.
6. preparation method according to claim 2, is characterized in that, the temperature of described sintering is 1000 DEG C ~ 1200 DEG C, and the time is 2 ~ 5 hours.
7. preparation method according to claim 2, is characterized in that, the temperature of described polarization is 80 DEG C ~ 120 DEG C, and the strength of electric field of polarization is 3kV/mm ~ 5kV/mm, and the time of polarization is 10 ~ 20 minutes.
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CN105732022A (en) * 2015-12-31 2016-07-06 中国科学院声学研究所 Preparation method of piezoelectric ceramic with high Curie temperature and film thereof
CN109851355A (en) * 2018-12-15 2019-06-07 扬州江嘉科技有限公司 Pyroelectric ceramic material and preparation method thereof
CN114621008A (en) * 2020-12-14 2022-06-14 中国科学院上海硅酸盐研究所 Multi-element lead zirconate titanate-based pyroelectric ceramic material and preparation method thereof

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