CN101670691B - 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 PDF

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CN101670691B
CN101670691B CN 200910160387 CN200910160387A CN101670691B CN 101670691 B CN101670691 B CN 101670691B CN 200910160387 CN200910160387 CN 200910160387 CN 200910160387 A CN200910160387 A CN 200910160387A CN 101670691 B CN101670691 B CN 101670691B
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翟继卫
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Tongji University
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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 is controlled 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 and can be used for a pyroelectric infrared detector, a smart device and a system.

Description

Anti-ferroelectric thin film used and the preparation that operation temperature area is adjustable and pyroelectric coefficient is larger
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 preparation method 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 preparation method and application technical field that adopts chemical method preparation to have adjustable working warm 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 abundant structure phase antiferroelectric near changing ferroelectric phase boundary into, and the 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 progress of modern surveying technology and the development of material phase structure and Characterization for Microstructure technology, the Structure property relationships when accurately measuring material and undergoing phase transition becomes possibility; And can utilize the electric field of antiferroelectric, temperature-induced phase transformation to realize switch and the adjusting of the various functions effects such as piezoelectricity, pyroelectricity, electric field induced strain, the research of materials 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℃ -1Such as 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-temp 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 larger pyroelectricity electric current under electric field action.Utilize applying bias to regulate and control the temperature of antiferroelectric-ferroelectric (AFE-FE) phase transformation, thereby realize to regulate, reversible pyroelectric effect.
Because the applied voltage of antiferroelectric ceramics block materials is higher, is generally tens kilovolts every centimetre, has limited the application of antiferroelectric ceramics body.Therefore, the filming of antiferroelectric ceramics is the important channel of realizing that materials is used.
At present anti-ferroelectric thin film used research is mainly concentrated on: the chemical composition of (1) material and synthesis condition are on the impact of film microstructure and phase structure; (2) film thickness, interface and electrode material on film antiferroelectric-impact of ferroelectric properties, electric field induced strain; Such 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 working warm 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 3Pb specifically 0.97La 0.02(Zr 0.75Sn 0.16Ti 0.09) O 3And near antiferroelectric and ferroelectric phase boundary but be in antiferroelectric Tetragonal when regional its pyroelectric property better.
Described anti-ferroelectric thin film used (Pb, Nb) (Zr, Sn, Ti) O 3Pb specifically 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 adopts 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 rotary coating method of compatibility prepare gel mould, then heat-treat, repeat this process, until obtain the film of desired thickness, prepare in its surface again one deck PbO gel mould, 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 respectively ethylene glycol ethyl ether, zirconium iso-propoxide Zr (OC 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 respectively ethylene glycol ethyl ether, ethanol niobium Nb (OC 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 rotary coating method of compatibility prepare gel mould, then carry out 450～550 ℃, 3～7 minutes heat treatment, repeat this process, until obtain the film of desired thickness, prepare in its surface again one deck PbO gel mould, 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 more intelligent.And have large 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 large pyroelectric coefficient at its transformation temperature place, and phase transition temperature is adjustable under the effect of applying bias voltage, has wide market prospects 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, the Nb) on/Si substrate (Zr, Sn, Ti) O 3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the graph of a relation of partially sending a telegraph pressure.
Fig. 2 is that preparation is at LaNiO 3/ Pt/Ti/SiO 2(Pb, the La) on/Si substrate (Zr, Sn, Ti) O 3Anti-ferroelectric thin film used pyroelectricity electric current and pyroelectric coefficient and temperature, add the graph of a relation of partially sending a telegraph pressure.
The specific embodiment
Be described in further detail below in conjunction with example, the example of lifting below being to be understood that does not comprise all the elements of the present invention just for the present invention that explains:
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 adopts 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 respectively ethylene glycol ethyl ether, ethanol niobium Nb (OC 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, adopts the method for rotary coating to prepare 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 lower one deck gel mould, 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 fully dissolving after adding glacial acetic acid, adds ethylene glycol also 110 ℃ of lower backflows 2 hours, 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.Film surface at the 820nm of front step preparation adopts the PbO precursor solution of 0.8M concentration to prepare one deck PbO gel mould again.
At last with this film 700 ℃ of lower heat treatments 30 minutes.Then the method sputter top electrode of d.c. sputtering is adopted on the surface thereon, and its diameter is that 0.5mm, thickness are about 100nm.Then the method sputter top electrode of d.c. sputtering is adopted on the surface thereon, and 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 partially sending a telegraph pressure.
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 to be in antiferroelectric Tetragonal regional.
The chemical raw material that adopts 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 respectively ethylene glycol ethyl ether, zirconium iso-propoxide Zr (OC 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, adopts the method for rotary coating to prepare 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 lower one deck gel mould, the film thickness that obtains for 15 times that moves in circles is 810nm, and then the PbO precursor solution that adopts in its surface 0.8M concentration prepares one deck PbO gel mould, at last with this film 700 ℃ of lower heat treatments 30 minutes.Then the method sputter top electrode of d.c. sputtering is adopted on the surface thereon, and its diameter is that 0.5mm, thickness are about 100nm.Then the method sputter top electrode of d.c. sputtering is adopted on the surface thereon, and 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 partially sending a telegraph pressure.
The concentration of used precursor solution, the number of plies of coating and last to obtain the total thickness of film relevant, namely molar concentration is larger, and its thickness is also just larger; The number of plies is more, and its thickness is also larger.For ferroelectric thin film, its thickness is 600-800nm generally speaking.

Claims (2)

1. one kind has the adjustable working warm area and has big pyroelectric coefficient at the transformation temperature place, and anti-ferroelectric thin film used as pyroelectricity material comprises: anti-ferroelectric thin film used Pb 0.99Nb 0.02(Zr 0.85Sn 0.13Ti 0.02) 0.98O 3With cover anti-ferroelectric thin film used Pb 0.99Nb 0.02(Zr 0.85Sn 0.13Ti 0.02) 0.98O 3The PbO gel mould on surface; This anti-ferroelectric thin film used Pb 0.99Nb 0.02(Zr 0.85Sn 0.13Ti 0.02) 0.98O 3The preparation of employing sol-gal process, substrate is LaNiO 3/ Pt/Ti/SiO 2/ Si, thickness are 600-800nm, and its preparation method comprises following two steps:
The preparation of a, precursor solution: the solute that adopts is lead acetate, ethanol niobium, tin acetate, zirconium iso-propoxide and isopropyl titanate, and solvent is glacial acetic acid, ethylene glycol ethyl ether and deionized 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 rotary coating method of compatibility prepare gel mould, then carry out 450～550 ℃, 3～7 minutes heat treatment, repeat this process, until obtain the film of desired thickness, prepare in its surface again one deck PbO gel mould, at last 650-700 ℃ of heat treatment 30～60 minutes; Anti-ferroelectric thin film used Pb 0.99Nb 0.02(Zr 0.85Sn 0.13Ti 0.02) 0.98O 3Be in the zone of antiferroelectric rhombic system.
2. a kind of anti-ferroelectric thin film used pyroelectricity film as infrared thermal release electric detector as pyroelectricity material claimed in claim 1.
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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
JP6264525B2 (en) * 2013-03-25 2018-01-24 セイコーエプソン株式会社 Infrared sensor, heat detection element, and heat detection method using the same
CN103641477B (en) * 2013-12-09 2015-04-15 华中科技大学 Anti-ferroelectric energy storage ceramic material and preparation method thereof
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
CN110981467B (en) * 2019-12-09 2020-12-29 华中科技大学 Lead-free pyroelectric composite ceramic material 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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