CN103641477B - Anti-ferroelectric energy storage ceramic material and preparation method thereof - Google Patents
Anti-ferroelectric energy storage ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an anti-ferroelectric energy storage ceramic material and a preparation method thereof. The anti-ferroelectric ceramic material is formed by compounding a tetragonal anti-ferroelectric phase in the mass fraction of k and an orthogonal anti-ferroelectric phase in the mass fraction of (1-k), wherein the tetragonal anti-ferroelectric phase is (Pb0.87-1.5xBa0.1La0.02Mx) (Zr0.95-ySnyTi0.05) O3, the orthogonal anti-ferroelectric phase is (Pb0.97La0.02) (Zr0.95-zSn0.05Tiz) O3, M is one of Y, Eu and Yb, x=0-0.015, y=0.25-0.45, z=0.03-0.05 and k=40%-60%. The preparation method comprises the following steps: (1) preparing tetragonal phase anti-ferroelectric ceramic powder; (2) preparing orthogonal phase anti-ferroelectric ceramic powder; (3) compounding the tetragonal phase anti-ferroelectric ceramic powder and the orthogonal phase anti-ferroelectric ceramic powder in mass percentage to obtain the anti-ferroelectric energy storage ceramic material. The anti-ferroelectric ceramic material can keep relatively high saturated polarization strength and simultaneously obtain a relatively large ferroelectric-anti-ferroelectric phase transition field so as to greatly improve the energy storage density.
Description
Technical field
The invention belongs to energy storage ceramic field of material technology, more specifically, relate to a kind of Anti-ferroelectric energy storage ceramic material and preparation method thereof.
Background technology
High energy storage density electric capacity plays more and more important role in various electric power, electronic system.Related electronic products is had higher requirement towards miniaturization, lightness and multifunctional direction development to capacitance energy storage density.The key improving electrical condenser energy storage characteristic is to develop the dielectric substance with high energy storage density.
At present, the dielectric substance of high density capacitors can be divided into four classes.The first kind is the material such as barium titanate, titanium dioxide, the production technology of associated capacitor is very ripe and be used widely, the feature of such material is that specific inductivity is very high, but be subject to the impact of defect (crystal boundary, hole etc.) and temperature in material, breaking down field strength is lower, and usual energy storage density is lower than 1J/cm
3.Equations of The Second Kind is organic film, and as polypropylene film, Mylar film (mylar), polyvinylidene difluoride (PVDF) (PVDF) film etc., feature is that breaking down field strength is very high, but specific inductivity is very little, use range critical constraints.3rd class is the composite dielectrics of pottery and polymkeric substance or glass, and this kind of material has the breaking down field strength of super general application far away, and mainly for pulse power system, and its mass production technology is still immature.4th class is antiferroelectric materials, and this kind of material has very high density (> 95%) and very little dielectric loss (< 1%).Under DC Electric Field, the rapid transformation of antiferroelectric → ferroelectric phase can be there is, specific inductivity shows strong non-linear effect, cause the linear or near-linear medium under the far super equality strength electric field action of its polarizability, therefore in mesolow range of application, the far advanced three class dielectric materials of its energy storage density, become the study hotspot of present stage.
The principal element affecting antiferroelectric materials energy storage density height has two: saturated polarization and ferroelectric-antiferroelectric phase variable field.Present stage, both at home and abroad the research of high energy storage density antiferroelectric materials is mainly concentrated on plumbous lanthanum zirconium tin titanium (PLZST) material of Tetragonal and orthorhombic phase PLZST material.Wherein, Tetragonal PLZST material have saturated polarization high, ferroelectric-feature that antiferroelectric phase variable field is little, be usually made into block ceramic research.Due to this system material ferroelectric-antiferroelectric phase variable field much smaller than its breaking down field strength, its energy storage density is generally at 2.5J/cm
3below.Compared with Tetragonal PLZST material, orthorhombic phase PLZST material ferroelectric-antiferroelectric phase variable field can reach level far above Tetragonal PLZST breakdown strength of material, energy storage density can up to 15J/cm
3.But the saturated polarization of orthorhombic phase PLZST material is on the low side, and is not suitable for energy storage ceramic field, and is applicable to energy storage film applications, and thus its energy storage total amount is restricted.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of Anti-ferroelectric energy storage ceramic material and preparation method thereof, while keeping higher saturated polarization, obtain larger ferroelectric-antiferroelectric phase variable field, thus the energy storage density of stupalith is largely increased.
For achieving the above object, according to one aspect of the present invention, provide a kind of Anti-ferroelectric energy storage ceramic material, it is characterized in that, be composited by the massfraction orthogonal antiferroelectric phase that to be the cubic antiferroelectric phase of k and massfraction be (1-k); Described cubic antiferroelectric phase is (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, described orthogonal antiferroelectric phase is (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, M is the one in Y, Eu and Yb, x=0 ~ 0.015, y=0.25 ~ 0.45, z=0.03 ~ 0.05, k=40% ~ 60%.
Preferably, x=0.006, y=0.3, z=0.05.
Preferably, k=45% ~ 50%.
According to another aspect of the present invention, provide a kind of preparation method of above-mentioned Anti-ferroelectric energy storage ceramic material, it is characterized in that, comprise the steps: that (1) prepares Tetragonal antiferroelectric ceramics powder: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, by mixture dry, sieve after heat-treat to obtain sintered material, again by sintered material ball mill pulverizing, drying, sieve, obtain Tetragonal antiferroelectric ceramics powder (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, wherein, x=0 ~ 0.015, y=0.25 ~ 0.45; (2) orthorhombic phase antiferroelectric ceramics powder is prepared: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, after mixture oven dry, sieving, at 850 ~ 900 DEG C synthesize 2 ~ 3 hours, then by synthetic material ball milling, drying, sieve, obtain orthorhombic phase antiferroelectric ceramics powder (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, z=0.03 ~ 0.05; (3) the orthorhombic phase antiferroelectric ceramics powder that the Tetragonal antiferroelectric ceramics powder described step (1) obtained and described step (2) obtain is prepared burden according to mass percent, granulation after stirring, and compression moulding, shaping base substrate is sintered 2 ~ 3 hours at 1240 ~ 1250 DEG C, and cooling after annealing 0.5 ~ 1 hour at 1050 ~ 1100 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Preferably, in described step (1), described heat treatment process is specially: synthesize 2 ~ 3 hours at prior to 850 ~ 900 DEG C, then by granulation after synthetic material ball mill pulverizing, sinters 2 ~ 3 hours after granulation material being filled alms bowl at 1220 ~ 1240 DEG C.
In general, the above technical scheme conceived by the present invention compared with prior art, by cubic antiferroelectric phase and orthogonal antiferroelectric phase by a certain percentage compound prepare Anti-ferroelectric energy storage ceramic material, while the cubic antiferroelectric phase height saturated polarization of maintenance, increased substantially cubic antiferroelectric phase ferroelectric-antiferroelectric phase variable field, thus energy storage density is greatly improved.
Accompanying drawing explanation
Fig. 1 is the crystal orientation composition of the Anti-ferroelectric energy storage ceramic material of the contrary ferroelectric ceramic powder content of different orthogonal of the embodiment of the present invention that records of XRD and comparative example;
Fig. 2 is the micro-structure diagram of the Anti-ferroelectric energy storage ceramic material of the contrary ferroelectric ceramic powder content of different orthogonal of the embodiment of the present invention that records of SEM and comparative example, and wherein, the mass percentage of (a) orthorhombic phase antiferroelectric ceramics powder is 40%; B the mass percentage of () orthorhombic phase antiferroelectric ceramics powder is 50%; C the mass percentage of () orthorhombic phase antiferroelectric ceramics powder is 60%;
Fig. 3 is the ferroelectric hysteresis loop figure of the Anti-ferroelectric energy storage ceramic material of the contrary ferroelectric ceramic powder content of different orthogonal of the embodiment of the present invention and comparative example, and wherein, the mass percentage of (a) orthorhombic phase antiferroelectric ceramics powder is respectively 0%, 40% and 50%; B the mass percentage of () orthorhombic phase antiferroelectric ceramics powder is respectively 55% and 60%.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
Anti-ferroelectric energy storage ceramic material of the present invention is composited by the massfraction orthogonal antiferroelectric phase that to be the cubic antiferroelectric phase of k and massfraction be (1-k).Wherein, cubic antiferroelectric phase is (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, orthogonal antiferroelectric phase is (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, M is the one in Y, Eu and Yb, x=0 ~ 0.015, y=0.25 ~ 0.45, z=0.03 ~ 0.05, k=40% ~ 60%.
Particularly, x=0.006, y=0.3, z=0.05.
The preparation method of Anti-ferroelectric energy storage ceramic material of the present invention comprises the steps:
(1) Tetragonal antiferroelectric ceramics powder is prepared: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, by mixture dry, sieve after heat-treat to obtain sintered material, again by sintered material ball mill pulverizing, drying, sieve, obtain Tetragonal antiferroelectric ceramics powder (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, wherein, x=0 ~ 0.015, y=0.25 ~ 0.45.
(2) orthorhombic phase antiferroelectric ceramics powder is prepared: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, after mixture oven dry, sieving, at 850 ~ 900 DEG C synthesize 2 ~ 3 hours, then by synthetic material ball milling, drying, sieve, obtain orthorhombic phase antiferroelectric ceramics powder (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, z=0.03 ~ 0.05.
(3) the orthorhombic phase antiferroelectric ceramics powder that Tetragonal antiferroelectric ceramics powder step (1) obtained and step (2) obtain is prepared burden according to mass percent, polyvinyl alcohol (PVA) granulation is added after stirring, type is made at 100MPa pressure, shaping base substrate is sintered 2 ~ 3 hours at 1240 ~ 1250 DEG C, and cooling after annealing 0.5 ~ 1 hour at 1050 ~ 1100 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Heat treatment process in above-mentioned steps (1) is specially: synthesize 2 ~ 3 hours at prior to 850 ~ 900 DEG C, then by after synthetic material ball mill pulverizing, add PVA granulation, sinters 2 ~ 3 hours after granulation material being filled alms bowl at 1220 ~ 1240 DEG C.
For making those skilled in the art understand the present invention better, below with cubic antiferroelectric phase (Pb
0.861ba
0.1la
0.02y
0.006) (Zr
0.65sn
0.3ti
0.05) O
3with orthogonal antiferroelectric phase (Pb
0.97la
0.02) (Zr
0.9sn
0.05ti
0.05) O
3(M is Y, x=0.006, y=0.3, z=0.05) is example, is described in detail in conjunction with specific embodiments to the preparation method of Anti-ferroelectric energy storage ceramic material of the present invention.
Embodiment 1
The preparation method of the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention comprises the steps:
(1) according to molecular formula (Pb
0.861ba
0.1la
0.02y
0.006) (Zr
0.65sn
0.3ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, dries mixture, sieves, reinstall quartz crucible, synthesize 3 hours at 850 DEG C, then synthetic material is poured into after pulverizing in ball grinder, to add mass percent be the concentration of 8wt% be 5% PVA granulation, at 1220 DEG C, sinter 3 hours after granulation material being filled alms bowl.Finally, sintered material is placed in ball grinder ball mill pulverizing, dry, sieve, obtain Tetragonal antiferroelectric ceramics powder.
(2) according to molecular formula (Pb
0.97la
0.02) (Zr
0.9sn
0.05ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, mixture is dried, sieved, reinstalls quartz crucible, synthesize 2 hours at 900 DEG C, then synthetic material poured into ball milling in ball grinder, drying, sieve, obtain orthorhombic phase antiferroelectric ceramics powder.
(3) the orthorhombic phase antiferroelectric ceramics powder 60:40(k=60% in mass ratio that Tetragonal antiferroelectric ceramics powder step (1) obtained and step (2) obtain) mix, to add mass percent be again the concentration of 8wt% is after the PVA granulation of 5%, type is made at 100MPa pressure, shaping base substrate is sintered 2 hours at 1250 DEG C, and furnace cooling after annealing 1 hour at 1050 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Embodiment 2
The preparation method of the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention comprises the steps:
(1) according to molecular formula (Pb
0.861ba
0.1la
0.02y
0.
006) (Zr
0.65sn
0.3ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, dries mixture, sieves, reinstall quartz crucible, synthesize 2.5 hours at 900 DEG C, then synthetic material is poured into after pulverizing in ball grinder, to add mass percent be the concentration of 8wt% be 5% PVA granulation, at 1240 DEG C, sinter 2.5 hours after granulation material being filled alms bowl.Finally, sintered material is placed in ball grinder ball mill pulverizing, dry, sieve, obtain Tetragonal antiferroelectric ceramics powder.
(2) according to molecular formula (Pb
0.97la
0.02) (Zr
0.9sn
0.05ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, mixture is dried, sieved, reinstalls quartz crucible, synthesize 2.5 hours at 900 DEG C, then synthetic material poured into ball milling in ball grinder, drying, sieve, obtain orthorhombic phase antiferroelectric ceramics powder.
(3) the orthorhombic phase antiferroelectric ceramics powder 50:50(k=50% in mass ratio that Tetragonal antiferroelectric ceramics powder step (1) obtained and step (2) obtain) mix, to add mass percent be again the concentration of 8wt% is after the PVA granulation of 5%, type is made at 100MPa pressure, shaping base substrate is sintered 3 hours at 1240 DEG C, and furnace cooling after annealing 0.5 hour at 1100 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Embodiment 3
The preparation method of the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention comprises the steps:
(1) according to molecular formula (Pb
0.861ba
0.1la
0.02y
0.006) (Zr
0.65sn
0.3ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, dries mixture, sieves, reinstall quartz crucible, synthesize 2 hours at 900 DEG C, then synthetic material is poured into after pulverizing in ball grinder, to add mass percent be the concentration of 8wt% be 5% PVA granulation, at 1240 DEG C, sinter 2 hours after granulation material being filled alms bowl.Finally, sintered material is placed in ball grinder ball mill pulverizing, dry, sieve, obtain Tetragonal antiferroelectric ceramics powder.
(2) according to molecular formula (Pb
0.97la
0.02) (Zr
0.9sn
0.05ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, mixture is dried, sieved, reinstalls quartz crucible, synthesize 3 hours at 850 DEG C, then synthetic material poured into ball milling in ball grinder, drying, sieve, obtain orthorhombic phase antiferroelectric ceramics powder.
(3) the orthorhombic phase antiferroelectric ceramics powder 45:55(k=45% in mass ratio that Tetragonal antiferroelectric ceramics powder step (1) obtained and step (2) obtain) mix, to add mass percent be again the concentration of 8wt% is after the PVA granulation of 5%, type is made at 100MPa pressure, shaping base substrate is sintered 2.5 hours at 1250 DEG C, and furnace cooling after annealing 0.8 hour at 1050 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Embodiment 4
(1) Tetragonal antiferroelectric ceramics powder is obtained by the method identical with embodiment 1.
(2) orthorhombic phase antiferroelectric ceramics powder is obtained for the method that embodiment 1 is identical.
(3) the orthorhombic phase antiferroelectric ceramics powder 40:60(k=40% in mass ratio that Tetragonal antiferroelectric ceramics powder step (1) obtained and step (2) obtain) mix, to add mass percent be again the concentration of 8wt% is after the PVA granulation of 5%, type is made at 100MPa pressure, shaping base substrate is sintered 2.8 hours at 1240 DEG C, and furnace cooling after annealing 0.6 hour at 1100 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
Comparative example
According to molecular formula (Pb
0.861ba
0.1la
0.02y
0.006) (Zr
0.65sn
0.3ti
0.05) O
3middle stoichiometric ratio takes each feed composition, amounts to 300g.Raw material is poured in ball grinder, add dehydrated alcohol 200g, wet ball grinding, evenly rear discharging to be mixed, mixture is dried, sieved, reinstall quartz crucible, synthesize 3 hours at 850 DEG C, then synthetic material is poured into after pulverizing in ball grinder, to add mass percent be the concentration of 8wt% be 5% PVA granulation, granulation material is made type in 100MPa pressure, shaping base substrate is sintered 3 hours at 1220 DEG C, obtains Tetragonal antiferroelectric ceramics.
Test the energy storage characteristic of the anti-ferroelectric energy storage ceramic that above-described embodiment and comparative example obtain, result is as shown in table 1.
The energy storage characteristic of the anti-ferroelectric energy storage ceramic of table 1 embodiment and comparative example
According to above-mentioned energy storage characteristic parameter, the test result of composition graphs 1 ~ 3, can obtain, and Anti-ferroelectric energy storage ceramic material of the present invention has following features:
(1) XRD shows, two kinds of principal crystalline phases in the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention all belong to perovskite structure, there is obvious dispersal behavior between two phase compositions; After orthorhombic phase content reaches 60%, there is a small amount of pyrochlore constitution composition.
(2) SEM shows, in the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention, two-phase densification combines, without obvious visible pore.
(3) along with the raising of orthorhombic phase content, the FE-AFE phase variable field of the Anti-ferroelectric energy storage ceramic material of the embodiment of the present invention is the trend of first increases and then decreases, but all far above Tetragonal antiferroelectric ceramics, thus energy storage density is greatly improved.
Anti-ferroelectric energy storage ceramic material of the present invention is not limited to above-described embodiment, and particularly, M is not limited to Y, and x is not limited to 0.006, y and is not limited to 0.3, z and is not limited to 0.05, k and is not limited to 60%, 50%, 45% and 40%.More generally, M is any one in Y, Eu and Yb, and x is the arbitrary value between 0 ~ 0.015, and y is the arbitrary value between 0.25 ~ 0.45, and z is the arbitrary value between 0.03 ~ 0.05, and k is the arbitrary value between 40% ~ 60%.Preferably, when orthorhombic phase mass percent is 50% ~ 55%, namely during k=45% ~ 50%, Anti-ferroelectric energy storage ceramic material of the present invention can obtain higher energy storage density.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. an Anti-ferroelectric energy storage ceramic material, is characterized in that, is composited by the massfraction orthogonal antiferroelectric phase that to be the cubic antiferroelectric phase of k and massfraction be (1-k);
Described cubic antiferroelectric phase is (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, described orthogonal antiferroelectric phase is (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, M is the one in Y, Eu and Yb, x=0 ~ 0.015, y=0.25 ~ 0.45, z=0.03 ~ 0.05, k=40% ~ 60%.
2. Anti-ferroelectric energy storage ceramic material as claimed in claim 1, is characterized in that, x=0.006, y=0.3, z=0.05.
3. Anti-ferroelectric energy storage ceramic material as claimed in claim 1 or 2, is characterized in that, k=45% ~ 50%.
4. the preparation method of Anti-ferroelectric energy storage ceramic material as claimed in claim 1, is characterized in that, comprise the steps:
(1) cubic antiferroelectric phase ceramic powder is prepared: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, by mixture dry, sieve after heat-treat to obtain sintered material, again by sintered material ball mill pulverizing, drying, sieve, obtain cubic antiferroelectric phase ceramic powder (Pb
0.87-1.5xba
0.1la
0.02m
x) (Zr
0.95-ysn
yti
0.05) O
3, wherein, x=0 ~ 0.015, y=0.25 ~ 0.45;
(2) orthogonal antiferroelectric phase ceramic powder is prepared: take each feed composition according to stoichiometric ratio, by the raw material mixing configured, add dehydrated alcohol, ball milling obtains uniform mixture, after mixture oven dry, sieving, at 850 ~ 900 DEG C synthesize 2 ~ 3 hours, then by synthetic material ball milling, drying, sieve, obtain orthogonal antiferroelectric phase ceramic powder (Pb
0.97la
0.02) (Zr
0.95-zsn
0.05ti
z) O
3, wherein, z=0.03 ~ 0.05;
(3) the orthogonal antiferroelectric phase ceramic powder that the cubic antiferroelectric phase ceramic powder described step (1) obtained and described step (2) obtain is prepared burden according to mass percent, granulation after stirring, and compression moulding, shaping base substrate is sintered 2 ~ 3 hours at 1240 ~ 1250 DEG C, and cooling after annealing 0.5 ~ 1 hour at 1050 ~ 1100 DEG C, obtain Anti-ferroelectric energy storage ceramic material.
5. preparation method as claimed in claim 4, it is characterized in that, in described step (1), described heat treatment process is specially: synthesize 2 ~ 3 hours at prior to 850 ~ 900 DEG C, again by granulation after synthetic material ball mill pulverizing, after granulation material being filled alms bowl, at 1220 ~ 1240 DEG C, sinter 2 ~ 3 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580322A (en) * | 2004-05-15 | 2005-02-16 | 华中科技大学 | Method for preparing strontium-barium titanate ferroelectric film |
| CN1990418A (en) * | 2005-12-29 | 2007-07-04 | 同济大学 | Anti-ferroelectric thin film used as thermoelectrical material and preparing method and use thereof |
| CN101670691A (en) * | 2005-12-29 | 2010-03-17 | 同济大学 | Antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and preparation method thereof |
| CN102432289A (en) * | 2011-09-21 | 2012-05-02 | 天津大学 | Iron-lanthanum-doped lead zirconate titanate antiferroelectric ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580322A (en) * | 2004-05-15 | 2005-02-16 | 华中科技大学 | Method for preparing strontium-barium titanate ferroelectric film |
| CN1990418A (en) * | 2005-12-29 | 2007-07-04 | 同济大学 | Anti-ferroelectric thin film used as thermoelectrical material and preparing method and use thereof |
| CN101670691A (en) * | 2005-12-29 | 2010-03-17 | 同济大学 | Antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and preparation method thereof |
| CN102432289A (en) * | 2011-09-21 | 2012-05-02 | 天津大学 | Iron-lanthanum-doped lead zirconate titanate antiferroelectric ceramic and preparation method thereof |
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