Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations

By RF magnetron sputtering method the Pt/PZT-film/Pt:Ti-sublayer/SiO₂/Si-substrate structures were prepared and pyroelectric response amplitude and phase behaviour under external voltage application was investigated by photopyroelectric modulation method. The results of investigation of pyroelectri...

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Опубліковано в: :Semiconductor Physics Quantum Electronics & Optoelectronics
Дата:2004
Автори: Bravina, S.L., Cattan, E., Morozovsky, N.V., Remiens, D.
Формат: Стаття
Мова:English
Опубліковано: Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України 2004
Онлайн доступ:https://nasplib.isofts.kiev.ua/handle/123456789/119121
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Цитувати:Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations / S.L. Bravina, E. Cattan, N.V. Morozovsky, D. Remiens // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2004. — Т. 7, № 3. — С. 263-271. — Бібліогр.: 27 назв. — англ.

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Digital Library of Periodicals of National Academy of Sciences of Ukraine
id nasplib_isofts_kiev_ua-123456789-119121
record_format dspace
spelling Bravina, S.L.
Cattan, E.
Morozovsky, N.V.
Remiens, D.
2017-06-04T15:58:22Z
2017-06-04T15:58:22Z
2004
Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations / S.L. Bravina, E. Cattan, N.V. Morozovsky, D. Remiens // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2004. — Т. 7, № 3. — С. 263-271. — Бібліогр.: 27 назв. — англ.
1560-8034
PACS: 78.20.-e
https://nasplib.isofts.kiev.ua/handle/123456789/119121
By RF magnetron sputtering method the Pt/PZT-film/Pt:Ti-sublayer/SiO₂/Si-substrate structures were prepared and pyroelectric response amplitude and phase behaviour under external voltage application was investigated by photopyroelectric modulation method. The results of investigation of pyroelectric response – external voltage loops of polarization reversal, pyroelectric response – voltage poling curves and pyroelectric response – time repolarization curves and also dynamic current-voltage characteristics of Pt/PZT/Pt:Ti/SiO₂/Si-substrate structures are presented. From variation of pyroelectric response in the current and voltage modes the capacity-voltage loops of polarization reversal and poling curves were derived. From asymmetric pyroelectric response – time repolarization curves the voltage behaviour of characteristic times of zero response and saturation was analyzed. Observed transformations of current-voltage characteristics display the considerable voltage and time dependent variation of charge transfer conditions. The performed investigation has shown the strong correlation between the poling pyroelectric and so ferroelectric and electrical asymmetries. Presented data on the polar and time asymmetry of the conditions of polarization reversal are discussed in the terms of influence of dynamics of space charge asymmetry on pinning conditions under the different polarity of applied voltage in the course of polarization reversal.
Authors gratefully acknowledge Ministry of Science of France and the University of Valenciennes for financial support.
en
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
Semiconductor Physics Quantum Electronics & Optoelectronics
Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
Article
published earlier
institution Digital Library of Periodicals of National Academy of Sciences of Ukraine
collection DSpace DC
title Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
spellingShingle Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
Bravina, S.L.
Cattan, E.
Morozovsky, N.V.
Remiens, D.
title_short Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
title_full Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
title_fullStr Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
title_full_unstemmed Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations
title_sort peculiarities and asymmetry of polarization reversal in pt/pzt-film/pt:ti/sio₂/si-substrate structures in pyroelectric response investigations
author Bravina, S.L.
Cattan, E.
Morozovsky, N.V.
Remiens, D.
author_facet Bravina, S.L.
Cattan, E.
Morozovsky, N.V.
Remiens, D.
publishDate 2004
language English
container_title Semiconductor Physics Quantum Electronics & Optoelectronics
publisher Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
format Article
description By RF magnetron sputtering method the Pt/PZT-film/Pt:Ti-sublayer/SiO₂/Si-substrate structures were prepared and pyroelectric response amplitude and phase behaviour under external voltage application was investigated by photopyroelectric modulation method. The results of investigation of pyroelectric response – external voltage loops of polarization reversal, pyroelectric response – voltage poling curves and pyroelectric response – time repolarization curves and also dynamic current-voltage characteristics of Pt/PZT/Pt:Ti/SiO₂/Si-substrate structures are presented. From variation of pyroelectric response in the current and voltage modes the capacity-voltage loops of polarization reversal and poling curves were derived. From asymmetric pyroelectric response – time repolarization curves the voltage behaviour of characteristic times of zero response and saturation was analyzed. Observed transformations of current-voltage characteristics display the considerable voltage and time dependent variation of charge transfer conditions. The performed investigation has shown the strong correlation between the poling pyroelectric and so ferroelectric and electrical asymmetries. Presented data on the polar and time asymmetry of the conditions of polarization reversal are discussed in the terms of influence of dynamics of space charge asymmetry on pinning conditions under the different polarity of applied voltage in the course of polarization reversal.
issn 1560-8034
url https://nasplib.isofts.kiev.ua/handle/123456789/119121
citation_txt Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO₂/Si-substrate structures in pyroelectric response investigations / S.L. Bravina, E. Cattan, N.V. Morozovsky, D. Remiens // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2004. — Т. 7, № 3. — С. 263-271. — Бібліогр.: 27 назв. — англ.
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AT morozovskynv peculiaritiesandasymmetryofpolarizationreversalinptpztfilmpttisio2sisubstratestructuresinpyroelectricresponseinvestigations
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first_indexed 2025-11-24T15:47:04Z
last_indexed 2025-11-24T15:47:04Z
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fulltext 263© 2004, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine Semiconductor Physics, Quantum Electronics & Optoelectronics. 2004. V. 7, N 3. P. 263-271. PACS: 78.20.-e Peculiarities and asymmetry of polarization reversal in Pt/PZT-film/Pt:Ti/SiO2/Si-substrate structures in pyroelectric response investigations S.L. Bravina, E. Cattan*, N.V. Morozovsky, D. Remiens* Institute of Physics NASU, 46, prospect Nauky, 03028 Kyiv, Ukraine E-mail: bravina@iop.kiev.ua * IEMN-DOAE- MIMM CNRS-UMR 8520, Universite de Valenciennes et du Hainaut- Cambresis, 9, Le Mont Houy, 59313 Valenciennes Cedex, France E-mail: denis.remiens@univ.valenciennes.fr Abstract. By RF magnetron sputtering method the Pt/PZT-film/Pt:Ti-sublayer/SiO2/Si-substrate structures were prepared and pyroelectric response amplitude and phase behaviour under external voltage application was investigated by photopyroelectric modulation method. The results of investigation of pyroelectric response � external voltage loops of polarization reversal, pyroelectric response � voltage poling curves and pyroelectric response � time repo- larization curves and also dynamic current-voltage characteristics of Pt/PZT/Pt:Ti/SiO2/Si- substrate structures are presented. From variation of pyroelectric response in the current and voltage modes the capacity-voltage loops of polarization reversal and poling curves were derived. From asymmetric pyroelectric response � time repolarization curves the voltage behaviour of characteristic times of zero response and saturation was analyzed. Observed transformations of current-voltage charac- teristics display the considerable voltage and time dependent variation of charge transfer conditions. The performed investigation has shown the strong correlation between the poling pyroelectric and so ferroelectric and electrical asymmetries. Presented data on the polar and time asymme- try of the conditions of polarization reversal are discussed in the terms of influence of dynam- ics of space charge asymmetry on pinning conditions under the different polarity of applied voltage in the course of polarization reversal. Keywords: PZT-film/Si structures, pyroelectric response hysteresis loops, polar and poling asymmetry. Paper received 20.05.04; accepted for publication 21.10.04. 1. Introduction Polar PZT ceramics are known as materials with excel- lent piezoelectric and pyroelectric properties [1, 2], which are retained in PZT films [3, 4]. A good technological compatibility with Si-base of modern electronics makes PZT films be a leader in creation of elements of high- density dynamic random access memories (DRAM�s), non-volatile random access memories (NV-RAM�s), mi- cro-electro-mechanics (MEM�s) and infrared sensorics (IRS's) [3�5]. The practically important electrical characteristics of �metal-PZT-film-metal on Si-substrate� system as those of other systems of such type manifest the well-known set of natural and technological asymmetries connected with specificity of reversing the poling state in the electroded ferroelectric film on the substrate [3�5]. The asymmetries of ferroelectric hysteresis loops and current-voltage characteristics were found not only for strongly asymmetric Au/PZT/Si heterojunction structures [6] and also for weak asymmetric Ni/PZT/Pt/Si struc- tures, which also possess the pyroelectric asymmetry [7]. Pyroelectricity is well known not only as important applicable effect [2] but also as a high informative method of the polar state investigation [8], especially when pyroelectric response amplitude and phase behaviour was investigated by photopyroelectric modulation method [8]. In this method the sample is investigated in the operation modes of pyroelectric detector of radiation (PDR). In this paper we present the results of investigations of polar and poling asymmetries of the set of pyroelectric 264 SQO, 7(3), 2004 S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... characteristics of Pt/PZT-film/Pt:Ti/SiO2/Si-substrate systems obtained by photopyroelectric modulation method. 2. Experimental 2.1. Samples The samples of PZT films were prepared by radio fre- quency magnetron sputtering method on platinized SiO2/Si substrate. The bottom Pt:Ti-bilayer was formed by platinum bottom electrode with a titanium adhesive layer (150 nm of Pt and 10 nm of Ti) deposited on 350 nm SiO2 layer on (100) n-type Si substrate. For substrate stabilization the annealing treatment of the Pt:TiOx/SiO2/Si-substrate structure just before of PZT deposition was performed at 350�400°C. Then PZT film was deposited on the bottom electrode. The sputter- ing target obtained by uniaxially cold pressing includes the mixture of PbO, TiO2 and ZrO2 in the stoichiometric composition. The polar perovskite phase of the PZT-film was obtained by post-annealing treatment at 600�650°Ñ during 0,5�1 hour. The top Pt-electrodes were deposited through a shadow mask by sputtering procedure, which was followed by a lift-off, and have ≈1 mm2 of area. The details of the sputtering conditions were described else- where [9, 10]. The obtained PZT-films with Zr/Ti ratio 54/46 are near the morphotropic phase boundary, which corre- sponds to better performances for bulk PZT ceramics. The thickness of the main components are the follow- ing: 150 nm for the top Pt-electrode, 1.9 µm for layer for PZT layer, 350 µm for Si substrate. Each element has a current-carrying thin stripe with a circle current electrode of 1 mm of diameter on the stripe end. 2.2. Measurements For the investigations of pyroelectric and ferroelectric characteristics the measuring set for complete pyroelectric and ferroelectric characterization [8] was used. The measurements of amplitude Uπ and phase ϕπ of pyroelectric response were carried out by photopyro- electric modulation method in the current and voltage modes. In the current mode Uπ = Uπ1 ∝ γ/c1, and in the voltage mode Uπ = Uπ2 ∝ γ/c1ε⋅fm, (here γ is the pyroelect- ric coefficient, c1 is the volume heat capacity, ε is the dielectric permittivity, fm is the modulation frequency) [2, 8]. Since Uπ1 ∝ γ and Uπ2 ∝ γ/ε, the dielectric ratio Dπ = Uπ1/Uπ2 fm ∝ επ reflects the behaviour of dielectric permittivity obtained by pyroelectric measurements. Under examination of loops of pyroelectric response hysteresis (Uπ -V-loops and ϕπ-V- loops) the Pt/PZT/Pt:Ti/ Si structure was investigated in the operating mode of ferroelectric bolometer, at that applied d.c. voltage Vdc was varied stepwise ±(0,25�1) V cyclically in the range of �10 V ≤ Vdc ≤ +10 V. The same mode was used under investigations of variations of transient pyroelectric re- sponse in due course under application of d.c. voltage (Uπ-t- and ϕπ-t- curves). The Uπ1,2-V-curves were obtained after previous pulse depoling of the samples up to zero response, which remains during a long period without poling voltage application. The Uπ-t-curves were obtained after previous 11 V d.c. poling of the samples up to satu- rated Uπ value, which remains during a long period with- out poling voltage application. For minimization of polarization reversal contribu- tion under dynamic current-voltage characterization (I�V-curves) the unipolar saw-tooth drive voltage Vd with 0,5 s of durability and 1 Hz of repetitive frequency in the amplitude range of 0 ≤ Vd ≤ 10 V was used. During pyroelectric measurements the structure un- der investigation was irradiated by modulated IR-probe from IR LED supplied by generator of sinusoidal vol- tage through the matching stage [8]. The matching stage for sensitive elements (SE) of PDR, based on FET impedance transformer with using dynamic load and changeable impedance in the input circuit was applied [11, 12]. It successively operates in the current mode (power measurement) and voltage mode (energy measurement) in the range from infrasound up to low ultrasound frequencies. So, the investigated Pt/PZT/ Pt:Ti/Si structures were placed in the conditions of op- eration of the real SE of PDR. 3. Results and comments 3.1. Pyroelectric response characteristics 3.1.1. Pyroelectric response � modulation frequency characteristics The dependences Uπ1,2(fm) and ϕπ1,2(fm), obtained for the investigated samples of Pt/PZT film/Pt:Ti/Si after posi- tive (�+�) and negative (���) d.c. poling are presented in Figures 1a and 1b. The shapes of Uπ1,2(fm) and ϕπ1,2(fm) are near identi- cal for �+� and ��� poled SE (compare Figs 1a and 1b). Consecutive repolarization of SE gives 180°-addition to ϕ1,2 which corresponds to the change of sign of pyro- electric reaction of PZT film and only insignificant vari- ations of shape of Uπ1,2(fm) and ϕπ1,2(fm) dependences. This indicates the almost complete pyroelectric revers- ibility of reorientation of polarization direction in inter- electrode space of Pt/PZT/Pt:Ti structure. A small scat- ter of Uπ1,2 values can be explained by the difference in the degree of unipolarity of PZT film under the top Pt electrode and the bottom Pt:Ti one. 3.1.2. Pyroelectric response � voltage poling curves Figure 1c presents the dependences of pyroelectric re- sponse value on the poling voltages lower than the coer- S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... 265SQO, 7(3), 2004 cive ones and also near them. The application of the ex- ternal d.c. voltage Vdc leads to the increase of Uπ1,2 from zero to saturated values. These saturated values increase with the increase of Vdc and remain during a long period after getting off the Vdc of both negative and positive polarities. Obtained Uπ1,2-V-curves display the asymmetry of positive and negative branches which consists in particu- lar in positive shift of zero response regions and the breaks in the vicinity of the threshold voltages Vth ±. Observed threshold inequality of Uπ1,2-V-curves (Vth � < Vth +) corre- sponds to the coercive inequality of Uπ1,2-V -loops (Vc �< < Vc +) (see part 3.1.3). For observed behaviour of ϕπ1,2-V-curves is charac- teristic 180°-change of ϕπ1,2 under change of Vdc polar- ity, which corresponds to the change of the sign of pyroelectric reaction under polarization reversal. Difference in Vth � and Vth + values (Vth � < Vth +) are visible under examination of the behavior of dielectric ratio � voltage curves (Dπ-V-curves) (Figure 1c). Since Dπ(Vdc) = Uπ1(Vdc)/Uπ2(Vdc) ∝ επ(Vdc) the Dπ(Vdc) depend- ency reflects the behavior of επ(Vdc). The tendency of changing Dπ(Vdc) observed on Dπ-V- curves indicates the decrease of επ(Vdc) under Vdc in- crease, which corresponds to decrease of the number of domain walls in the film under poling. The peculiarities of positive and negative branches of Dπ-V-curves around of Vth ± are more diffused for Vth � than for Vth +. This re- flects some differences in rearrangements of domain struc- ture of the Pt/PZT film/Pt:Ti/SiO2/Si systems under dif- ferent polarities of external voltage. 10 0 10 1 10 2 10 3 10 4 10 5 10 0 101 102 103 i a P y ro el ec tr ic r es p o n se Up1 /Up2 ⋅f Up2, µV Up1, µV 10 0 10 1 10 2 10 3 10 4 10 5 Modulation frequency, Hz P h a se , d e g . �100 0 100 200 300 i jp2 jp1 b P y ro e le c tr ic r es p o n se , V m 10 0 10 1 10 2 10 3 10 4 10 5 10 0 101 102 103 Up1 /Up2 ⋅f Up2, µV Up1, µV h P h a se , d e g . �100 0 100 200 300 10 0 10 1 10 2 10 3 10 4 10 5 jp2 jp1 Modulation frequency, Hz h Fig. 1. Modulation frequency dependences (a, b) and poling curves (c) of pyroelectric response amplitudes Uπ1,2(fm), dielec- tric ratio Dπ = Uπ1/Uπ2 fm and phases ϕπ1,2(fm): a � after +35 V, 5 min d.c. poling; b � after �35 V, 5 min d.c. poling. c � under d.c. poling after complete depoling. c P y ro e le ct r ic , V m P h a se , d eg . D ie l. r a ti o , a . u . 0 5 10 15 20 D.C. voltage, V 20 Hz �6 �6 �6 �5 �5 �5 �4 �4 �4 �3 �3 �3 �2 �2 �2 �1 �1 �1 0 0 0 1 1 1 2 2 2 3 3 3 4 4 4 5 5 5 6 6 6 �100 0 100 200 300 1400 1600 1800 2000 2200 =D Up p1 / U ~ep2 Up2, µV Up1, µV j p2 jp1 266 SQO, 7(3), 2004 S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... 3.1.3. Pyroelectric response � external voltage poling � repoling loops In Figures 2a and 2b the obtained loops of pyroelectric response amplitude |Uπ1,2(Vdc)| and phase ϕπ1,2(Vd) and also their combination into real signal Uπ1,2(Vdc) are pre- sented. The |Uπ1,2|-V-loops have the typical �butterfly�-like shape, which is often observed for strain-electric field response loops of PZT films [13]. The behaviour of |Uπ1,2(Vdc)| is characterized by the regions of saturation at the front of the �wings� where Vd > Vc and sharp changes with pronounced minima on the �tails� of the �wings� in the vicinity of Vd = Vc. The ϕπ1,2-V-loops have the characteristic parallelo- gram-like shape with the regions of ϕπ1,2-change on 180° in the vicinity of Vdc = Vc and ϕπ(Vdc) = const outside the range of Vd = Vc. Symmetry of the front parts of both positive and nega- tive |Uπ1,2(Vdc)| � �wings� reflects the pyroelectric iden- tity of both polarized states of investigated PZT film. Asymmetry of the �tails� of the |Uπ1,2(Vdc)| � �wings� and inequality Vc � < Vc + indicates the difference on the ear- lier stage of repolarization processes. The shapes of obtained Uπ1,2-V-loops and inequa- lity Vc � < Vc + in general are similar to that known for P-V-loops of metal/PZT-film/Si-substrate system [3, 4, 7, 9, 13]. The analysis of Uπ1-V-loops and Uπ2-V-loops shows earlier and more complete saturation of Uπ1(Vdc) poling curves comparatively with undersaturated Uπ2(Vdc) poling curves for the both of Vdc polarities. Since Uπ1 ∝ γ and Uπ2 ∝ γ/ε, we can conclude that the saturation of γ value starts just before Vc ± and finishes just after Vc ±, which is earlier than that of γ/ε value. So this is the ε value which remains undersaturated under Vdc > Vc ±. The behavior of dielectric ratio Dπ(Vdc) ∝ επ(Vdc) is reflected by Dπ-V-loop presented in Figure 2c. Observed asymmetry of Dπ-V-loop corresponds to the same of the Uπ1,2(Vdc) -loops. The general view of obtained Dπ(Vdc) changes under poling-repoling cycle reflects the general tendency of decreasing επ value in the poling run under Vdc increase and conservation of lower value of επ under subsequent decrease of Vdc. Also the step-like jumps of Dπ(Vdc) in vicinity of Vdc = 0 with the maxima around of Vdc = 0 are observed. The sharp peculiarities of Dπ(Vdc) around of Vdc = Vc are visible and the first one at Vc + is more pronounced than the second one at Vc �. These peculiarities of Dπ(Vd) reflect the variations of επ(Vd) and so the states of the domain structure of PZT film with the near zero unipo- larity degree. The behaviour of επ(Vdc) in the vicinity of Vdc = 0 and Vdc = Vc ± can be connected with the peculiarities of rear- rangement of domain structure of PZT film which con- sists in mutual transformations of interconnected 180°- and non-180°- (in particular, 90°-) domain groups [5, 14]. 3.1.4. Pyroelectric response � time repolarization transient curves Figure 3 presents the changes of pyroelectric response amplitude and phase in the course of repolarization of Pt/PZT film/Pt:Ti structure by application of d.c. volt- age Vdc less and near the coercive ones. Under application of fixed external repoling d.c. volt- age Vdc the decrease of Uπ value up to zero followed by subsequent increase of Uπ value up to saturated one is observed. This saturated value remains during a long period after Vdc getting off. Observed behaviour of ϕπ(t), namely 180°-change un- der transition of Uπ(t) through its zero value, corresponds to the change of the sign of pyroelectric reaction due to polarization reversal in time induced by Vdc application. For positive and for negative Vdc the similar tendency in the Uπ(t) behaviour but at different time scales is ob- served. So the strong asymmetry in the time scale of repolarization process development is clearly evident. Figure 4 presents repolarization transient curves Uπ(t) combined from amplitude and phase time dependences from Figure 3. For positive and for negative poling voltages the re- gions of Uπ(t) ~ Uπ(0)(1 � ηlog(t/τ)) are observed and the slope η increase with Vdc value increase. For negative Vdc on the both sides from zero response time the view of Uπ(t) is different at low Vdc and similar at high Vdc. So under negative Vdc the characteristics of domain walls motion before and after repolarization are different at low Vdc values and are similar at high Vdc values. For positive Vdc on the both sides from zero response time the slopes of Uπ(t) are different at both low and high Vdc. So, under positive Vdc the characteristics of domain walls motion before and after repolarization are different at low and high Vdc values. In Figure 5 the voltage dependences of zero-response time t0 and saturation time ts are presented. Increase of negative Vdc value leads to strong decrease of ts and t0 values, which remain near constant when Vdc value reaches and exceeds the Vc � value. Under positive Vdc value the same tendency of t0 changing but in more narrow time scale is observed. At low Vdc the values of t0 are 1�2 orders of value higher at negative Vdc than at positive ones but at high Vdc for the both polarities the values of to are near the same. Under increase of negati- ve Vdc the ts value decreases similar to t0 but under increa- se of positive Vdc the ts value noticeably increases. So, for negative Vdc the similar tendencies and for positive Vdc the different tendencies in the behaviour of t0 and ts are observed. 3.2. Dynamic unipolar current-voltage characteristics Figure 6 presents the set of dynamic unipolar current- voltage characteristics obtained under different ampli- tudes and polarities of drive voltage. S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... 267SQO, 7(3), 2004 In general, the structure of considered dynamic I�V- curves is similar to those quasistatic ones observed for many other electroded PZT-film based structures obtained by different technologies [15�17]. On the I�V-curves ob- tained at Vd < Vc can be distinguished three characteris- tic regions. The first one at low Vd values is short and jump-like and is connected with displacement current in the moment of Vd rise. The second one at intermediate Vd values is sub-linear. The third one at high Vd values is super-linear. The voltages Vt � and Vt + of transition between sub- linear and super-linear regions increase with increasing Vd amplitude. Comparison of the data in Figure 6 shows that the differences of positive and negative branches which in- crease with the rise of Vd values are rather high at short times of Vd application and decrease after forming under long term repetitive action of Vd saw-pulses. So observed dynamic I�V-curves shows a pronounced dynamic char- acter of polar asymmetry. For unformed I�V-curves the development of super- linear region with the rise of Vd is characteristic. The forming during several minutes leads to the changes of �15 �10 -5 0 5 10 15 0.1 1 10 100 20 Hz a P y ro el e ct r ic r e sp o n se A m p li tu d e , V µ U U p p 2 1 �15 �10 -5 0 5 10 15 -100 0 100 200 300 V , V = P h a se , d eg . jp2 jp1 �15 �10 -5 0 5 10 15 V , V= �30 �20 �10 0 10 20 30 20 Hz b P y ro e le c tr ic r e sp o n se , V µ Up2 �15 �10 -5 0 5 10 15 V ,V = �3 �2 �1 0 1 2 3 20 Hz P y r o e le c tr ic r e sp o n se , V µ Up1 �15 �10 -5 0 5 10 15 1000 1200 1400 1600 1800 2000 D.c. voltage, V D ie le c tr ic R a ti o , a r b . u n it s 20 Hz c =D Up p1 / U f ~ ⋅ e p2 Fig. 2. Pyroelectric response � d.c. voltage loops: a � �butterflies� of amplitudes Uπ1,2(V), and parallelograms of phases 1,2(V); b � hysteresis loops of responses Uπ2(V) (top) and Uπ1(V) (bot- tom); c � dielectric ratio Dπ(V) loop. 268 SQO, 7(3), 2004 S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... parameters of the I�V-curves. These changes are more significant under increasing the drive voltage value (com- pare the data in Figure 6). The expansion of sub-linear region at the expense of super-linear one are observed. Under Vd increase the slope of sub-linear region de- creases. Under Vd > Vc the appearance of region with the diffuse maximum and subsequent negative slope is char- acteristic and more pronounced for the positive branch. These regions are connected with currents of polariza- tion reversal in the definite group of domains (�stubborn domains�) which spontaneously return in the initial state under Vd = 0. Taking into account the complex character of mixed 90°- and 180°- domain structure in PZT films [5] and the data [14] concerning the contribution of 180°- and non-180°-domain groups into remanent polarization in PZT films we can suppose that the stubborn domain group in a significant degree consists of non-180°-do- mains. 4. Discussion The obtained results show that the investigated systems possess polar asymmetry of pyroelectric parameters, poling time and current-voltage characteristics, which correspond to coexistence of interrelated ferroelectric asymmetry and asymmetry of charge transport. Indeed, processes of polarization reversal in the Pt/PZT/Pt:Ti/TiO2/SiO2/Si structures are developed in the condition of asymmetry of injection properties of Pt- top and Pt:Ti-bottom contacts due to the difference in the conditions of their manufacturing. Besides, there is an asymmetry of profile of the space charge connected with the profile of mobile and immobile point and expanded defects. In PZT films these are VPb + and VO � vacancies, domain walls, boundaries of separate micro-regions of PZT film, and also various types of distortions in under- electrode regions of the film. In the case of investigated Pt/PZT/Pt:Ti structures, because of the complex configuration of the space charge, the charge transport on the different stages of repo- larization process can be realized by so called relay- race alternation of different mechanisms (see their list in Ref [17]). The complex structure of observed I�V-curves and its changes in time are in accordance with this inter- pretation. Time, s d.c. voltage: +4 V +4.5 V +5 V +6 V 10 0 10 10 1 1 10 10 2 2 10 10 3 3 10 10 4 4 10 10 5 5 0.0 0.0 0.5 0.5 1.0 1.0 1.5 1.5 2.0 2.0 2.5 2.520 Hz d.c. voltage: �4 V �4.5 V �4.75 V �5 V �5.5 V �6 V 10 10 5 5 10 10 4 4 10 10 3 3 10 10 2 2 10 10 1 1 10 10 10 0 0 0 �100 �100 0 0 100 100 200 200 P h a se , d e g . P y ro el ec tr ic r e sp o n se A m p li tu d e , V µ Fig. 3. Pyroelectric response amplitude-time and phase-time repolarization curves: top � pyroelectric response amplitude; bottom � pyroelectric response phase; left � for negative d. c. voltages; right � for positive d. c. voltages. Time, s 10 0 10 1 10 2 10 3 10 4 10 5 10 5 10 4 10 3 10 2 10 1 10 0 P y ro e le ct ri c re sp o n se A m p li tu d e , V µ d.c. voltage: +4 V +4.5 V +5 V +6 V �2 �2 �1 �1 0 0 1 1 2 2 3 3 20 Hzd.c. voltage: �4 V �4.5 V �4.75 V �5 V �5.5 V �6 V Fig. 4. Pyroelectric response signal � time repolarization tran- sient curves: left � for negative d. c. voltages; right � for positive d. c. voltages. �7 �6 �5 �4 �3 10 100 0 10 101 1 10 102 2 10 103 3 10 104 4 Voltage, V C h a r a ct e r is ti c ti m e s, s 3 4 5 6 7 t s t o Fig. 5. Voltage dependences of pyroelectric response charac- teristic times under d. c. voltage repolarization: left � for nega- tive d. c. voltages: right � for positive d. c. voltages. S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... 269SQO, 7(3), 2004 �2 �1 0 1 2 �15 �10 �5 0 5 10 15 1 Hz saw pulses 10 s 1�3 min Current density, µA/cm2 Voltage, V �60 �40 �20 0 20 40 60 1 Hz saw pulses Voltage, V �6 �3 0 3 6 10 s 2-3 min Current density, µA/cm2 �8 �4 0 4 8 �80 �60 �40 �20 0 20 40 60 1 Hz saw pulses 10 s 1 min 3 min Voltage ,V Current density, µA/cm2 �80 �100 �60 �40 �20 0 20 40 60 1 Hz saw pulses Voltage ,V �10 �5 0 5 10 10 s 1 min 3 min Current density, µA/cm2 Fig. 6. Dynamic unipolar current-voltage characteristics under different drive voltage amplitudes. 270 SQO, 7(3), 2004 S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... A super-linear region of I�V curves is usually associ- ated with enrichment with charge carriers of near-con- tact region with metal and discussed in terms of injection mechanisms connected with the existence of currents lim- ited by space charge [18], Schottky emission [19] and Pool-Frenkel ionization [20]. A sub-linear region of I-V- curves can be connected with depletion of contacting re- gions of essentially different degree of doping due to ex- clusion and extraction of charge carriers [21]). The for- mation of such structure is characteristic for the case of diffusion of metal in semiconductor in the region of their contact as the result of thermal treatment and is quite possible in the course of manufacturing the investigated Pt/PZT/Pt:Ti structures. Dynamic character of observed current asymmetry points to the change of conditions of charge transport with time. So, the observed pyroelectric asymmetry is developed in the conditions of changing the space charge profile with time. The changes of pyroelectric response under reversing polarization are connected with domain structure recon- struction. That is why the time of such changes is deter- mined in a high degree with processes of nucleation of new domains and displacement of domain walls. The peculiarities of domain structure behaviour un- der polarization direction reversal in the perovskite crys- talline ferroelectrics [22] and in PZT films [5, 14, 23] are similar in many details. For initially non-polarized or depolarized crystals and PZT films, contained a number of disordered domains of non-180°- (in particular, 90°-) and 180°- orientation the polarization process occurs under action of external voltage by simultaneous displace- ment of non-180°- and 180°- domain boundaries, and reorientation of 180°-domains. The process of polariza- tion reversal in PZT films starts from the nucleation and growth of opposite domains (OD) of wedge-like shape from the surface into the depth of the film and finishes by broadening the domains spreading through the film by side displacement of domain walls (DW). The role of processes of charge transport under po- larization reversal in thin layer structures of metal- ferroelectric-metal type by means of formation OD and displacement of charged DW was considered earlier in [24, 25]. Facilitation of the conditions of domain nuclea- tion and growth in film structures due to presence of di- electric non-uniformity was considered recently in [26, 27]. To provide the displacement of charged DW it is necessary to supply the certain value of mobile electric charges, which is necessary for compensation of change- able bounded charge. The peculiarities of this DW dis- placement define the peculiarities of Uπ-V- and Uπ-t- curves. Under registration of Uπ-V- poling curves the increase of Uπ(Vdc) from zero value to the maximal one at given Vdñ value starts in the system of mutually pyroelectrically compensated ÎD and occurs in the system of rearranged ÎD. At that the value Vdñ = Vth corresponds to the begin- ning of sharp change of Uπ under Vdñ increase and so the start of fast rearrangement in the system of OD. Under registration of Uπ-t-curves of repolarization the variation of Uπ(t) reflects the trend of compensation process in the preliminary arranged OD system. The moment t = t0 when Uπ(t0) = 0 corresponds to pyro- electrically compensated state of OD system. So the time t = t0 corresponds to transport of such value of electrical charge, which is necessary for creation of number of ÎD required for compensation. The fact of vanishing Uπ values at Vd = Vc ± under Uπ- V-loops cycling and also at t = t0 ± under Uπ-t-curves re- gistration permits to consider some analogies between the coercive voltages Vc ± and zero response times t0 ±. Starting from the definition of the effective degree of unipolarity ξ = (ñ+ � ñ�)/(ñ+ + ñ�), where ñ+ and ñ� are the concentrations of the domains with the opposite direc- tions of the components of polarization vector Ps along the thickness of the film, we can conclude that at Vd = Vc ± and at t = t0 ± the value ξ = 0. Since the values Vd = Vc ± and t = t0 ± correspond to the similar states of the domain structure, namely those just balanced between two in- versely poled states, we can consider t0 as the coercive times. Indeed, from the standpoint of transport of charge value necessary for vanishing the value of integral po- larization, the coercive voltage is the necessary voltage value under given time of its action, and the coercive time is the necessary time under given voltage value. 5. Conclusions The performed investigation has shown the strong corre- lation between the poling pyroelectric and so ferroelectric and electrical asymmetries. Observed behaviour of Uπ-V- and Uπ-t-curves and also Uπ-V-loops displays the considerable polar and time asymmetry of polarization reversal. Observed transformation of I�V-curves is the evidence of considerable V- and t- dependent variation of charge transport conditions. Changes of pinning conditions, domain wall motion characteristics, charge and mechanical state of the point (immobile and mobile) and extended (domain wall) de- fects is the reason of observed complex asymmetry. For the investigated PZT thin films on Si systems with complex composition and asymmetric space charge pro- file is characteristic its change with time under the action of applied external voltage. The consequence of contact asymmetry and space charge asymmetry is the difference in the conditions of electric charge transport under the different polarity of applied voltage. It results, in particular, in different time of space charge accumulation necessary for reversing the polarization direction and also in different spread of this process in time. It leads to the difference in coercive times for Uπ-t-curves obtained under different polarity of poling voltage, and also to the difference in coercive voltage values obtained for Uπ1-V- and Uπ2-V-loops under differ- ent polarity of drive voltage. For as more complete as possible examination of po- larization reversal processes in PZT thin films on Si struc- S.L. Bravina et al.: Peculiarities and asymmetry of polarization reversal in ... 271SQO, 7(3), 2004 tures it is necessary to perform the investigation of the complex of their electrophysical characteristics includ- ing not only ferroelectric but at the least pyroelectric and current-voltage characteristics. Acknowledgements Authors gratefully acknowledge Ministry of Science of France and the University of Valenciennes for financial support. References 1. B. Jaffe, W. R. Cook, H. Jaffe, Piezoelectric ceramics, Acad. Press., London, 1971. 2. L.S. Kremenchugsky and O.V. Roitsina, Pyroelectric Detec- tors of Radiation, Naukova Dumka, Kiev, 1979 (in Russian). 3. Y. Ishibashi, Ferroelectric Thin Films: Synthesis and Basic Properties, Gordon and Breach, Amsterdam, pp. 135-152, 1996. 4. V.Y. Shur, Ferroelectric Thin Films: Synthesis and Basic Prop- erties, Gordon and Breach, Amsterdam, pp. 153-169, 1996. 5. R. Waser, Modeling of electroceramics � application and prospects // J. Europ. Ceram. Soc., 19, pp. 655-664 (1999). 6. Y. Xu, C. J. Chen, R. Xu, J. D. Mackenzie, Self biased heterojunction effect of ferroelectric thin film on silicon // Ferroelectrics, 108(1-4), pp. 47-52 (1990). 7. W. Liu, J. Ko, W. Zhu, Asymmetric switching behavior of Ni/ Pb1,1(Zr0,3Ti0,7)O3/Pt thin films // Material Letters, 49, p. 122 (2001). 8. S.L. Bravina, N.V. Morozovsky, A.A. Strokach, Pyroelec- tricity: Some Physical and Application Aspects // Proceed- ings of SPIE, 3182, pp. 85-99 (1997). 9. G. Velu, D. Remiens and B. Tierry, Ferroelectric properties of PZT thin films prepared by sputtering with stoichiometric single oxide target: comparison between conventional and rapid thermal annealing // J. Europ. Ceram. Soc., 17, p. 1749 (1997). 10. T. Haccart, E. Kattan, D. Remiens, Dielectric, ferroelectric and piezoelectric properties of sputtered PZT thin films on Si substrates: influence of film thickness and orientation // Semicond. Phys., Quant. Electron. and Optoelectronics, 5(1), pp. 78-88 (2002). 11. N.V. Morozovsky , V.B. Samoilov, I.A. Stoyanov, Investiga- tion of matching stages for pyroelectric detectors of radia- tion, in book Thermal Detectors of Radiation, GOI, Lenin- grad, pp. 104-105 (1980). 12. S.L. Bravina, L.S. Kremenchugsky, N.V. Morozovsky et.al., Investigation of Phase Transitions in Ag3AsS3 and Ag3SbS3 by Method of Dynamic Pyroelectric Effect, Preprint No. 26, Inst. of Phys. of Acad. Sci. of Ukraine, Kiev, 1982 (in Rus- sian). 13. P. Pertsch, M.-J. Pan, V. R. Vedula, S. Yoshikawa, S.-E. Park, T.R. Shrout, Characteristics of electromechanical solid state multilayer actuators // IEEE, pp. 571-574 (1998). 14. K. Saito, T. Oikawa, T. Kurosawa, T. Akai and H. Funakubo, Role of non-180o domain switching in electrical properties of Pb(Zr0.35Ti0.65)O3 thin films // Jpn. J. Appl. Phys., 41, Part 1, No 11B, pp. 6730-6734 (2002). 15. H. Miki, K. Kushida-Abdelghafar, K. Torii, Y. Fujisaki, Hydrogen related degradation and recovery phenomena in Pb(Zr,Ti)O3 capacitors with a platinum electrode // Jpn. J. Appl. Phys., 36, Part 1, No. 3A, pp. 1132-1135 (1997). 16. M. Brazier, M. McElfresh, S. Mansour, Origin of anomalous polarization offsets in compositionally graded Pb(Zr,Ti)O3 thin films // Appl. Phys. Lett., 74(2), pp. 299-31 (1999). 17. Stolichnov and A. Tagantsev, Space-charge influenced- ingection model for conduction in Pb(ZrxTi1�x)O3 thin films // J. Appl. Phys., 84(6), pp. 3216-3225 (1998). 18. M. A. Lampert and P. Mark, Current Injection in Solids, Academic, New-York, 1970. 19. W. Monch ed., Electronic Structureof Metal-Semiconductor Contacts, Kluwer Academic, Dordrecht, 1990. 20. F.F. Volkenshtein, Electrical Conductivity of Semiconduc- tors, Òåchtåîrizdat, Ìîscow-Låningrad, 1947 (in Russian). 21. V.L. Bonch-Brujevitch, S.G. Kalashnikov, Physics of Semi- conductors, Nauka, Moscow, 1977. 22. E.G. Fesenko, V.G. Gavriliatshenko, A.F. Sementshev, Do- main structure of multi-axes ferroelectrics, Ed. of Rostov. Univ., Rostov-on-Don, 1990 (in Russian). 23. D. Fu, K. Suzuki, K. Kato, M. Minakata, H. Suzuky, Investigztion of domain switching and retention in orienta- ted PbZr0,3Ti0,7O3 thin film by scanning force microscopy // Jpn. J. Appl. Phys., 41, Part 2, No. 11B, pp. 6724-6729 (2002). 24. G.Ì. Guro, I.I. Ivanchik, N.F. Kovtoniuk, C-Domain Crystal BaTiO3 in the Short Circuited Capacitor // Sov. Sol. St. Phys., 11(7), pp. 1956-1964 (1969). 25. V. F. Krapivin and Å. V. Chensky, Space Charge Limited Currents in the system Metal-Ferroelectric-Metal // Sov. Sol. St. Phys., 12(2), pp. 597-604 (1970). 26. A. M. Bratcovsky, A. P. Levaniuk, Abrupt appearance of the pattern and fatigue of thin ferroelectric films // Phys. Rev. Lett., 84(14), pp. 3177-3180 (2000). 27. A. M. Bratcovsky, A. P. Levaniuk, Ease polarization switch- ing in ferroelectrics // Phys. Rev. Lett., 8(1), pp. 4614-4617 (2000).