CN101670691A - Antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and preparation method thereof - Google Patents
Antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antiferroelectric film with adjustable working temperature zone and higher pyroelectric coefficient and a preparation method and application thereof. The antiferroelectric film (Pb,Nb)(Zr,Sn,Ti)O3 taken as the pyroelectric material is prepared by a sol gel method, the solute of precursor solution can be lead acetate, lanthanum acetate or niobium ethoxide, stannic acetate, zirconium isopropoxide and titanium isopropoxide, the solvent includes glacial acetic acid, ethylene glycol ethyl ether, acetylacetone and water, the final concentration of the precursor solution iscontrolled between 0.2-0.4 M, and the substrate comprises LaNiO3/Pt/Ti/SiO2/Si and Pt/Ti/SiO2/Si. The antiferroelectric film is high in thermally stimulated current and adjustable in temperature andcan be used for a pyroelectric infrared detector, a smart device and a system.
Description
The application is to be on December 29th, 2005 applying date, and application number is 200510112416.3, and denomination of invention is: as dividing an application of anti-ferroelectric thin film used and its production and application the Chinese patent application of pyroelectricity material.
Technical field
The invention belongs to a kind of anti-ferroelectric thin film used and its production and application technical field that adopts chemical method preparation to have adjustable operation temperature area, big pyroelectric coefficient.
Background technology
The antiferroelectric state of antiferroelectric materials (AFE) can be ferroelectric state (FE) by the role transformation of temperature, electric field and pressure.Owing to have the abundant structures phase near changing ferroelectric phase boundary into antiferroelectric, and outfields such as temperature, stress and electric field cause that spontaneous polarization changes and produce cholesteric-nematic transition, therefore the research from antiferroelectric to the ferroelectric phase boundary region are laid particular emphasis on transformation behavior always and utilize the field induced phase transition effect to carry out this two broad aspect of power conversion.
In recent years along with the development of modern surveying development of technology and material phase structure and micro-structural characterization technique, structure when accurately measuring material and undergoing phase transition and the relation between the performance become possibility; And can utilize the electric field of antiferroelectric, temperature-induced phase transformation to realize the switch and the adjusting of all multifunctional effects such as piezoelectricity, pyroelectricity, electric field induced strain, the research of this type of material is that the application of infrared thermal release electric detector, alert and resourceful device and system lays the first stone.The middle and later periods nineties is at research antiferroelectric ceramics material (Pb, La) (Zr, Sn, Ti) O
3Find that between ferroelectric state and antiferroelectric state, record a very large pyroelectricity electric current, its pyroelectric coefficient can reach 10 during (PLZST) pyroelectricity characteristic
-6C/cm
2℃
-1As document Yang Tongqing, Liu Peng, XuZhuo, Zhang Liangying, YaoXi, Ferroelectrics, 230, shown in (1999) 181-186, this numerical value is Pb (Zr, Ti) O
3(PZT) between ceramic low temperature ferroelectric phase FER (L) and the high temperature ferroelectric phase FER (H) during phase transformation 10 times of pyroelectric coefficient; The warm area of antiferroelectric-ferroelectric phase transition is very wide simultaneously, is the phase transformation pyroelectricity material that a class gets a good eye DEVELOPMENT PROSPECT therefore.Induce antiferroelectric and ferroelectric state between will cause the pyroelectricity current peak during phase transformation, this is the coefficient result in electric field and temperature field.To general ferroelectric material, its pyroelectricity electric current I=(dPr/dT); But for antiferroelectric materials, its pyroelectricity electric current then is I=(dPr/dT)+Einduced (E of d ε/dT), second pyroelectricity electric current of then inducing for the applying direct current place.Obviously, compare with general ferroelectric material, antiferroelectric materials has bigger pyroelectricity electric current under electric field action.Utilize applying bias to regulate and control, thereby realize to regulate, reversible pyroelectric effect the temperature of antiferroelectric-ferroelectric (AFE-FE) phase transformation.
Because the applied voltage of antiferroelectric ceramics block materials is generally tens kilovolts every centimetre than higher, has limited the application of antiferroelectric ceramics body.Therefore, the filming of antiferroelectric ceramics is the important channel of realizing that this type of material is used.
At present anti-ferroelectric thin film used research is mainly concentrated on: chemical composition of (1) material and synthesis condition are to the influence of film microstructure and phase structure; (2) film thickness, interface and electrode material to film antiferroelectric-influence of ferroelectric properties, electric field induced strain; As document Baomin Xu, Paul Moses, Neelesh G.Pai, and L.Eric Cross, Appl.Phys.Lett., 72, (1998) 593-395 and Baomin Xu, L.Eric Cross, Jonathan J.Bernstein, Thin Solid Films, 377, shown in (2000) 712-718 etc.And the expression behaviour of some critical phenomena, particularly pyroelectricity during to anti-ferroelectric thin film used undergoing phase transition does not also go deep into, systematic research and exploitation.
At present to ferroelectric-para-electric, ferroelectric-ferroelectric between pyroelectricity material research more of phase transformation, to antiferroelectric-that the ferroelectric phase transition pyroelectric effect is then studied is less, and all concentrate in the antiferroelectric ceramics block materials, and also do not see report for anti-ferroelectric thin film used pyroelectricity research.
Summary of the invention
One of purpose of the present invention provides a kind of the anti-ferroelectric thin film used of adjustable operation temperature area, big pyroelectric coefficient that have.
Another object of the present invention provides above-mentioned this anti-ferroelectric thin film used preparation method.
A further object of the invention is the above-mentioned this anti-ferroelectric thin film used purposes of explanation.
Anti-ferroelectric thin film used (Pb, La) (Zr, Sn, Ti) O as pyroelectricity material of the present invention
3Or (Pb, Nb) (Zr, Sn, Ti) O
3It adopts the sol-gal process preparation, the solute of precursor solution is lead acetate, lanthanum acetate La or ethanol niobium, tin acetate, zirconium iso-propoxide and isopropyl titanate, solvent is glacial acetic acid, ethylene glycol ethyl ether, acetylacetone,2,4-pentanedione and water, the ultimate density of precursor solution is controlled between the 0.2-0.4M, and substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si and Pt/Ti/SiO
2/ Si.
Described anti-ferroelectric thin film used (Pb, La) (Zr, Sn, Ti) O
3Specifically be Pb
0.97La
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3And its pyroelectric property is better near antiferroelectric and ferroelectric phase boundary but when being in antiferroelectric cubic alpha region.
Described anti-ferroelectric thin film used (Pb, Nb) (Zr, Sn, Ti) O
3Specifically be Pb
0.99Nb
0.02(Zr
0.85Sn
0.13Ti
0.02)
0.98O
3And its pyroelectric property is better when being in antiferroelectric rhombic system regional.
Anti-ferroelectric thin film used preparation method as pyroelectricity material of the present invention is:
The preparation of a, precursor solution: the solute that is adopted is lead acetate, lanthanum acetate La or ethanol niobium, tin acetate, zirconium iso-propoxide and isopropyl titanate, solvent is glacial acetic acid, ethylene glycol ethyl ether, acetylacetone,2,4-pentanedione and water, and the ultimate density of precursor solution is controlled between the 0.2-0.4M;
The preparation of b, gel mould: adopt with semiconductor technology mutually the rotation painting method of compatibility prepare gel mould, heat-treat then, repeat this process, film up to obtaining desired thickness prepares one deck PbO gel mould, more in its surface at last 650-700 ℃ of heat treatment.
To (Pb, La) (Zr, Sn, Ti) O
3System, the concrete steps of preparation precursor solution are: at first with lead acetate Pb (CH
3COO)
23H
2O and lanthanum acetate La (CH
3COO)
3H
2O adds a certain amount of glacial acetic acid by the stoichiometric proportion weighing, is heated to 110 ℃ and refluxes 1 hour; Add tin acetate Sn (CH after being cooled to room temperature
3COO)
4And continue to reflux 1 hour; Add ethylene glycol ethyl ether, zirconium iso-propoxide Zr (OC respectively after being cooled to room temperature
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4And be heated to 110 ℃ and refluxed 1 hour; Add deionized water and glacial acetic acid after being cooled to room temperature, the concentration that makes the precursor solution that is synthesized is 0.2-0.4M.
To (Pb, Nb) (Zr, Sn, Ti) O
3System, the preparation of precursor solution: at first with lead acetate Pb (CH
3COO)
23H
2O adds a certain amount of glacial acetic acid by the stoichiometric proportion weighing, is heated to 110 ℃ and refluxes 1 hour; Add tin acetate Sn (CH after being cooled to room temperature
3COO)
4And continue to reflux 1 hour; Add ethylene glycol ethyl ether, ethanol niobium Nb (OC respectively after being cooled to room temperature
2H
5)
5, zirconium iso-propoxide Zr (OC
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4And be heated to 110 ℃ and refluxed 1 hour; Add deionized water and glacial acetic acid after being cooled to room temperature, the concentration that makes the precursor solution that is synthesized is 0.2-0.4M.
The detailed process of step b is: adopt with semiconductor technology mutually the rotation painting method of compatibility prepare gel mould, carry out 450～550 ℃, 3～7 minutes heat treatment then, repeat this process, up to the film that obtains desired thickness, prepare one deck PbO gel mould more in its surface, at last 650-700 ℃ of heat treatment 30～60 minutes.
PLZST and PNZST as pyroelectricity material of the present invention is anti-ferroelectric thin film used under the effect of applying bias voltage, can realize the adjusting to its phase transition temperature.Anti-ferroelectric thin film used to PLZST, with the increase of applying bias voltage, the switch temperature of its pyroelectricity increases; Anti-ferroelectric thin film used to PNZST, with the increase of applying bias voltage, the switch temperature of its pyroelectricity reduces.Therefore, can regulate the switch temperature scope of pyroelectric coefficient by the change of applying bias voltage, and then regulate the operating temperature of infrared thermal release electric detector, make it intelligent more.And have big pyroelectric coefficient because this class is anti-ferroelectric thin film used at its transformation temperature place, thereby can improve the sensitivity of infrared thermal release electric detector.
PLZST and PNZST as pyroelectricity material of the present invention is anti-ferroelectric thin film used, utilizes the sol-gel method preparation of chemistry, and production technology is simple; What make anti-ferroelectric thin film usedly has big pyroelectric coefficient at its transformation temperature place, and phase transition temperature is adjustable under the effect of applying bias voltage, has vast market prospect in the application of infrared thermal release electric detector.
Description of drawings
Fig. 1 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2(Pb, Nb) (Zr, Sn, Ti) O on the/Si substrate
3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the graph of a relation of sending a telegraph pressure partially.
Fig. 2 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2(Pb, La) (Zr, Sn, Ti) O on the/Si substrate
3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the graph of a relation of sending a telegraph pressure partially.
The specific embodiment
Be described in further detail below in conjunction with example, the example of being lifted below being to be understood that does not comprise all the elements of the present invention just in order to explain the present invention:
Embodiment 1
To (Pb, Nb) (Zr, Sn, Ti) O
3System is selected Pb
0.99Nb
0.02(Zr
0.85Sn
0.13Ti
0.02)
0.98O
3(PNZST) be in the zone of antiferroelectric rhombic system.
The chemical raw material that is adopted is for being lead acetate Pb (CH
3COO)
23H
2O, ethanol niobium Nb (OC
2H
5)
5, tin acetate Sn (CH
3COO)
4, zirconium iso-propoxide Zr (OC
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4, solvent is glacial acetic acid, ethylene glycol ethyl ether and deionized water.At first with lead acetate Pb (CH
3COO)
23H
2O adds a certain amount of glacial acetic acid by the stoichiometric proportion weighing, and the mol ratio of Pb and glacial acetic acid is 1: 10, is heated to 110 ℃ and refluxes 1 hour; Add tin acetate Sn (CH after being cooled to room temperature
3COO)
4And continue to reflux 1 hour; Add ethylene glycol ethyl ether, ethanol niobium Nb (OC respectively after being cooled to room temperature
2H
5)
5, zirconium iso-propoxide Zr (OC
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4, (Zr+Ti+Nb) mol ratio with ethylene glycol ethyl ether is 1: 10, and is heated to 110 ℃ of backflows 1 hour; Add deionized water and glacial acetic acid after being cooled to room temperature, (Zr+Ti+Nb) mol ratio with water is 1: 12, and it is 0.3M that the adding glacial acetic acid makes the concentration of precursor solution.
Employed substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si (100) and Pt/Ti/SiO
2/ Si, LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.
Getting molar concentration is the above-mentioned precursor solution of 0.3M, and the method that adopts rotation to apply prepares film, and rotary speed is 3000 rev/mins, 15 seconds time.Gel mould is directly put into 500 ℃ tube furnace, was placed 5 minutes, is cooled to room temperature after the taking-up, applies one deck gel mould down, and the film thickness that obtains for 15 times that moves in circles is 820nm.
Take by weighing a certain amount of lead acetate Pb (CH
3COO)
23H
2O is heated to 110 ℃ to dissolving fully after adding glacial acetic acid, adds ethylene glycol and also refluxes 2 hours down at 110 ℃, and the volume ratio of glacial acetic acid and ethylene glycol is 4: 1, and to make the molar concentration of its solution be 0.8M, is cooled to the PbO precursor solution that room temperature is synthesized 0.8M.On the film surface of the 820nm of preceding step preparation, adopt the PbO precursor solution of 0.8M concentration to prepare one deck PbO gel mould again.
At last with this film 700 ℃ of following heat treatments 30 minutes.The surperficial thereon then method sputter top electrode that adopts d.c. sputtering, its diameter is that 0.5mm, thickness are about 100nm.The surperficial thereon then method sputter top electrode that adopts d.c. sputtering, its diameter is that 0.5mm, thickness are about 100nm.
Fig. 1 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Pb on the/Si substrate
0.99Nb
0.02(Zr
0.85Sn
0.13Ti
0.02)
0.98O
3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the relation of sending a telegraph pressure partially.
Embodiment 2
To (Pb, La) (Zr, Sn, Ti) O
3System is selected Pb
0.97La
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3(PLZST) near antiferroelectric and ferroelectric phase boundary but be in antiferroelectric cubic alpha region.
The chemical raw material that is adopted is for being lead acetate Pb (CH
3COO)
23H
2O, lanthanum acetate La (CH
3COO)
3H
2O, tin acetate Sn (CH
3COO)
4, zirconium iso-propoxide Zr (OC
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4, solvent is glacial acetic acid, ethylene glycol ethyl ether and deionized water.
At first with lead acetate Pb (CH
3COO)
23H
2O and lanthanum acetate La (CH
3COO)
3H
2O adds a certain amount of glacial acetic acid by the stoichiometric proportion weighing, and (Pb+La) mol ratio with glacial acetic acid is 1: 10, is heated to 110 ℃ and refluxes 1 hour; Add tin acetate Sn (CH after being cooled to room temperature
3COO)
4And continue to reflux 1 hour; Add ethylene glycol ethyl ether, zirconium iso-propoxide Zr (OC respectively after being cooled to room temperature
3H
7)
4With isopropyl titanate Ti (OC
3H
7)
4, (Zr+Ti) mol ratio with ethylene glycol ethyl ether is 1: 10, and is heated to 110 ℃ of backflows 1 hour; Add deionized water and glacial acetic acid after being cooled to room temperature, (Zr+Ti) mol ratio with water is 1: 12, and it is 0.3M that the adding glacial acetic acid makes the concentration of precursor solution.
Employed substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si (100) and Pt/Ti/SiO
2/ Si, LaNiO
3, Pt, Ti, SiO
2With the thickness of Si sheet be respectively 150nm, 150nm, 50nm, 150nm and 3500nm.
Getting molar concentration is the above-mentioned precursor solution of 0.3M, and the method that adopts rotation to apply prepares film, and rotary speed is 3000 rev/mins, 15 seconds time.Gel mould is directly put into 500 ℃ tube furnace, was placed 5 minutes, be cooled to room temperature after the taking-up, apply one deck gel mould down, the film thickness that obtains for 15 times that moves in circles is 810nm, and then the PbO precursor solution that adopts 0.8M concentration in its surface prepares one deck PbO gel mould, at last with this film 700 ℃ of following heat treatments 30 minutes.The surperficial thereon then method sputter top electrode that adopts d.c. sputtering, its diameter is that 0.5mm, thickness are about 100nm.The surperficial thereon then method sputter top electrode that adopts d.c. sputtering, its diameter is that 0.5mm, thickness are about 100nm.
Fig. 2 is that preparation is at LaNiO
3/ Pt/Ti/SiO
2Pb on the/Si substrate
0.97La
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the relation of sending a telegraph pressure partially.
The concentration of used precursor solution, the number of plies of coating and last to obtain the total thickness of film relevant, promptly molar concentration is big more, and its thickness is also just big more; The number of plies is many more, and its thickness is also big more.For ferroelectric thin film, its thickness is 600-800nm generally speaking.
Claims (4)
1, a kind of operation temperature area is adjustable and that pyroelectric coefficient is bigger is anti-ferroelectric thin film used, comprising: anti-ferroelectric thin film used Pb
0.97Nb
0.02(Zr
0.758n
0.16Ti
0.09) O
3With cover anti-ferroelectric thin film used Pb
0.97Nb
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3The PbO gel mould on surface; This anti-ferroelectric thin film used Pb
0.97Nb
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3The preparation of employing sol-gal process, the solute of precursor solution is lead acetate, lanthanum acetate, tin acetate, zirconium iso-propoxide and isopropyl titanate, and solvent is glacial acetic acid, ethylene glycol ethyl ether and water, and the ultimate density of precursor solution is controlled between the 0.2-0.4M, and substrate is LaNiO
3/ Pt/Ti/SiO
2/ Si, anti-ferroelectric thin film used Pb
0.97Nb
0.02(Zr
0.75Sn
0.16Ti
0.09) O
3Near antiferroelectric and ferroelectric phase boundary but be in antiferroelectric cubic alpha region.
2, a kind of operation temperature area as claimed in claim 1 is adjustable and that pyroelectric coefficient is bigger is anti-ferroelectric thin film used, it is characterized in that: anti-ferroelectric thin film used Pb
0.97Nb
0.02(Zr
0.738n
0.16Ti
0.09) O
3Thickness be 600-800nm.
3, the anti-ferroelectric thin film used preparation method that the described arbitrary operation temperature area of claim 1～2 is adjustable and pyroelectric coefficient is bigger, this method comprises following two steps:
The preparation of a, precursor solution: the solute that is adopted is lead acetate, lanthanum acetate, tin acetate, zirconium iso-propoxide and isopropyl titanate, and solvent is glacial acetic acid, ethylene glycol ethyl ether and water, and the ultimate density of precursor solution is controlled between the 0.2-0.4M;
The preparation of b, glued membrane: adopt with semiconductor technology mutually the rotation painting method of compatibility prepare gel mould, carry out 450～550 ℃, 3～7 minutes heat treatment then, repeat this process, up to the film that obtains desired thickness, prepare one deck PbO gel mould more in its surface, at last 650-700 ℃ of heat treatment 30～60 minutes.
4, the anti-ferroelectric thin film used pyroelectricity film that the described a kind of operation temperature area of claim 1 is adjustable and pyroelectric coefficient is bigger as infrared thermal release electric detector.
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| CN102241511A (en) * | 2010-05-11 | 2011-11-16 | 中国科学院上海硅酸盐研究所 | Ferroelectric-antiferroelectric (FE-AFE) phase change pyroelectric ceramic material, ceramic element thereof and preparation methods of material and element |
| CN102241511B (en) * | 2010-05-11 | 2013-10-30 | 中国科学院上海硅酸盐研究所 | Ferroelectric-antiferroelectric (FE-AFE) phase change pyroelectric ceramic material, ceramic element thereof and preparation methods thereof |
| CN104075810A (en) * | 2013-03-25 | 2014-10-01 | 精工爱普生株式会社 | Infrared sensor, heat sensing element, and heat sensing method using the same |
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| CN103641477A (en) * | 2013-12-09 | 2014-03-19 | 华中科技大学 | Anti-ferroelectric energy storage ceramic material and preparation method thereof |
| CN103641477B (en) * | 2013-12-09 | 2015-04-15 | 华中科技大学 | Anti-ferroelectric energy storage ceramic material and preparation method thereof |
| CN104538539A (en) * | 2014-12-25 | 2015-04-22 | 内蒙古科技大学 | Electrocaloric effect refrigeration composite thick film material |
| CN104538539B (en) * | 2014-12-25 | 2017-06-27 | 内蒙古科技大学 | A kind of electric card effect refrigeration composite thick film material |
| CN110981467A (en) * | 2019-12-09 | 2020-04-10 | 华中科技大学 | Lead-free pyroelectric composite ceramic material and preparation method thereof |
| CN111233470A (en) * | 2020-01-20 | 2020-06-05 | 同济大学 | Antiferroelectric ceramic material with excellent charge and discharge performance and preparation method thereof |
| CN111233470B (en) * | 2020-01-20 | 2021-05-11 | 同济大学 | Antiferroelectric ceramic material with excellent charge and discharge performance and preparation method thereof |
| CN112142464A (en) * | 2020-09-17 | 2020-12-29 | 广西大学 | Preparation method of Nb-doped PZST-based relaxation antiferroelectric film through frequency regulation |
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