2830 IEEE TRANSACTIONS ON PLASMA SCIENCE, VOL. 41, NO. 10, OCTOBER 2013

Magnetoresistance Relaxation in Thin La-Sr-Mn-OFilms Exposed to High-Pulsed Magnetic Fields

Nerija Žurauskiene, Member, IEEE, Saulius Balevicius, Senior Member, IEEE, Dainius Pavilonis,Voitech Stankevic, Skirmantas Keršulis, and Jurij Novickij

Abstract— Presented are the results of an investigationof colossal magnetoresistance relaxation in nanostructuredLa-Sr-Mn-O films after the removal of the magnetic field pulse.400-nm thick films grown by the metal–organic chemical vapordeposition technique are studied in the magnetic field range of2–10 T and a temperature range of 100–290 K using a pulsedmagnetic field generator based on a capacitor bank discharge.A magnetic coil of special design with a nonmetallic outer casingmade from polyamide materials allowed us to distinguish therelaxation processes occurring during three different time scales:ultrafast (<1 µs), fast (∼100 µs), and slow (∼1 ms). The dynamicsof the fast relaxation is analyzed using the Kolmogorov–Avrami–Fatuzzo model, considering the reorientation of the magneticdomains into their equilibrium state. The slow relaxationis analyzed using the Kohlrausch–Williams–Watts modelconsidering the short-range interaction of the magnetic momentsin disordered grain boundaries having spin-glass properties.

Index Terms— Colossal magnetoresistance, magnetic fieldeffects, magnetic field sensors, manganites, resistance relaxationprocesses, thin films.

I. INTRODUCTION

THE renewed interest in doped polycrystalline manganitesduring the last decade was motivated by an increased

understanding of the fundamental properties of the colos-sal magnetoresistance (MR) phenomenon and its potentialapplication in various devices [1]. It is demonstrated thatpolycrystalline manganite films can be successfully used forthe development of B-scalar sensors operating in wide mag-netic field and temperature ranges. These are able to measurethe magnitudes of high-pulsed magnetic fields of millisecondduration in very small volumes. Such sensors are used tomeasure the magnetic diffusion processes in railguns [2],the distribution of highly inhomogeneous transient magneticfields during coilgun experiments [3], and in the magneticfields of nondestructive dual-coil pulsed-field magnets upto megagauss [4]. However, for plasma science, destructive

Manuscript received November 30, 2012; revised February 12, 2013;accepted April 23, 2013. Date of publication July 3, 2013; date of currentversion October 7, 2013. Research conducted in the scope of the EuropeanPulsed Power Laboratories known as the EPPL. This work was supported bythe Research Council of Lithuania under Grant MIP-062/2012.

N. Žurauskiene, S. Balevicius, D. Pavilonis, V. Stankevic, and S. Keršulisare with Semiconductor Physics Institute, Center for Physical Sciences andTechnology, Vilnius LT-01108, Lithuania (e-mail: zurausk@pfi.lt; sbal@pfi.lt;dainius.pavilonis@gmail.com; wstan@pfi.lt; skyrma@pfi.lt).

J. Novickij is with Vilnius Gediminas Technical University, Vilnius LT-03227, Lithuania (e-mail: jurij.novickij@vgtu.lt).

Color versions of one or more of the figures in this paper are availableonline at http://ieeexplore.ieee.org.

Digital Object Identifier 10.1109/TPS.2013.2261558

single-coil magnets, superconductive fault current limiters,and other applications, sensors measuring magnetic fields athigher than tens of kilohertz frequencies and operating at lowtemperatures are required. In such cases, it is important toavoid the magnetic memory effects that limit the speed of suchsensors. Thus, the investigation of these magnetic relaxationprocesses and the appropriate definition of their mechanismsin manganite films are of great importance.

Magnetic relaxation upon removal or reversal of theexternal magnetic field is studied in bulk and in filmmagnetic materials. Therefore, there are numerous papersproposing different mathematical expressions that can beused to characterize the time-dependences of the magne-tization and the resistance relaxation: logarithmic, power-law-like, exponential (Debye), stretched or compressed expo-nential. These all depend on the mechanisms involved[5]–[7]. The most important process for many magneticdevice applications is the slow relaxation process, whichrefers to timescales far longer than the 10−9 − 10−11 sfor spin-lattice interactions and the 10−11 − 10−13 s forspin–spin interactions [5]. Usually such slow relaxation isinvestigated in the time range of 10−2 − 104 s due to the lackof a capability to take faster measurements. Thus differentrelaxation mechanisms are used to explain this phenomenon:spin-glass-like behavior, the reorientation of ferromagneticdomains, transformation between the ferromagnetic and non-ferromagnetic phases, local disorder, and others [5]. It isdemonstrated that because of the close relation between thetransport properties and the magnetization of manganites, mea-surements of their resistance relaxation provide an excellentindirect method for the investigation of the magnetic relaxationphenomena in these materials [8].

In this paper, we present the results of an investigation ofcolossal MR relaxation in nanostructured La-Sr-Mn-O filmsgrown by the metal–organic chemical vapor deposition tech-nique.

II. EXPERIMENTAL SETUP

The La0.83Sr0.17MnO3 (LSMO) films, having thicknesses of400 nm, are deposited using the pulsed injection metal organicchemical vapor deposition technique onto a polycrystallinelucalox (99.9% Al2O3 + 0.1% MgO) substrate. Because ofthe polycrystalline structure of the substrate, polycrystallinefilms with a slight texture are produced. This is confirmedby reflection high-energy electron diffraction measurements.

0093-3813 © 2013 IEEE

ŽURAUSKIENE et al.: MAGNETORESISTANCE RELAXATION IN THIN La-Sr-Mn-O FILMS 2831

Fig. 1. (a) AFM profiles. (b)–(d) Images of the surfaces of films grownat different deposition conditions and having different average dimensionsD of the clusters. The obtained D and Tm values are indicated at each image.

The films are grown at different deposition conditions (chang-ing deposition temperature Td in the range of 700–750 °C)to obtain films with different average dimensions D of thecrystallite clusters. The morphology of the films is investigatedusing atomic force microscopy (AFM) (Fig. 1). These AFMprofiles demonstrated the complex structure of our films:crystallites with dimensions of 10–20 nm are cumulated inlarger clusters. Three different films having different D ofthe clusters are picked for the investigation: 1) 285 nm;2) 240 nm; and 3) 190 nm. The samples are fabricated incoplanar shapes onto which two 0.5 × 0.5 mm square Agelectrodes are deposited by thermal evaporation. These areseparated by a distance of 50 μm. The resistivity ρ dependenceon temperature is investigated by using a low dc electric fieldin a closed cycle helium gas cryo-cooler in the temperaturerange 5–300 K. The dependence revealed transition that istypical for manganites, i.e., from metal-like to an insulator-likestate at temperature Tm . The Tm and corresponding resistivityρm for the three films are as follows: 1) 245 K, 0.8 � ·cm; 2)240 K, 1.6 � ·cm; and 3) 235 K, 1.9 � ·cm. The MR mea-surements are performed in the temperature range of 100–290K using a pulsed magnetic field generator based on capacitorbank discharge through a multishot magnetic field coil.

A special nondestructive (at least 100 pulses) coil is con-structed for the MR relaxation experiments. The coil is woundwith 4.20 × 2.37 mm2 Cu-Nb microcomposite wire (conduc-tivity 65% IACS, strength UTS = 1.2 GPa, manufacturer—Boshvar Institute, Moscow), insulated with Kapton film andreinforced with Zylon fiber-epoxy composite. It consisted of40 turns (10 in each layer) with inner diameter of 14 mm,outer diameter of 34 mm, and length of 48 mm (Fig. 2).To avoid a tail of the magnetic field pulse after the currentis switched off, we fabricated a nonmetallic outer casingmade from polyamide material that allowed us to produce

Fig. 2. Measurement setup and schematic diagram of magnetic field coil.

Fig. 3. Magnetic field pulse (left scale) and resistivity change during thispulse (right scale).

0.9-ms duration half sine waveform magnetic field pulses withamplitudes of up to 10 T (see Fig. 3, left scale). The coilprepared in this manner is mounted into a double-walled,10-mm thick steel container for safety. The inner container isprecooled with liquid nitrogen. During the experiments, threemanganite samples together with a pick-up coil used for themagnetic field measurements are placed in the center of thisnondestructive coil. The signal from the pick-up coil is mea-sured by oscilloscope and recalculated to magnetic inductancevalues. The magnetic field is applied to the manganite filmplane parallel to the current direction. Each manganite sampleis connected through a twisted pair cable to three independentmeasurement devices (B-meters, see Fig. 2). A 6.2-k� ballastresistor (RB) is connected in series to the each sample havingresistance RS . The total voltage drop across both resistors(RB + RS) is 2.5 V. During experiment, the output voltagescorresponding to each sample’s change of resistance duringthe magnetic field pulse are stored in the internal memory ofthe B-meter and transferred to the PC on software packagerequest. For this purpose, the B-meters are connected usinga duplex fiber optic data link to a hub that transformed and

2832 IEEE TRANSACTIONS ON PLASMA SCIENCE, VOL. 41, NO. 10, OCTOBER 2013

encoded the data to one single USB signal and sent it throughUSB to the PC. The resistance relaxation after the magneticfield pulse is switched off (Fig. 3, right scale) is investigatedat various temperatures and magnetic fields. The time instantof switching off the field can be clearly seen by the spike inthe resistivity curve at 0.9 ms (it is also seen in the magneticinduction curve). It is related with interference generated byclosing of the thyristor in the current oscillating circuit ofcapacitor bank-magnetic field coil system.

III. RESULTS AND DISCUSSION

The typical resistivity dynamics of these manganite filmsafter the application of a 0.9-ms duration magnetic field pulsewith an amplitude of 6.3 T is shown in Fig. 3. One cansee that the relaxation processes occur in three different timescales: ultrafast (<1 μs), which follows the magnetic fieldpulse; fast (∼100 μs) and slow (∼1 ms) that occur after themagnetic field pulse is switched off. For the developmentof magnetic field sensors, it is important to determine theconditions under which the fast and slow relaxation com-ponents can be minimized to ensure sufficient measurementaccuracy. The results of this resistance (conductance) relax-ation, namely, the temperature and magnetic field dependencesof the time constants and remanent amplitudes of theseprocesses, are presented and analysed below using the well-known Kolmogorov–Avrami–Fatuzzo (KAF) and Kohlrausch–Williams–Watts (KWW) models [5].

A. KAF Model

The typical conductivity relaxation of the La-Sr-Mn-Ofilms, which we characterized as fast and measured at lowtemperatures (ferromagnetic state), is shown in Fig. 4. Thetime instant t = 0 is chosen as the moment when the magneticfield pulse is switched off (see Fig. 3). The conventional Debyerelaxation (exponential function) cannot be applied to fit theexperimental results. Thus the results are fitted to the onedescribing a compressed exponential decay [5]

σ(t) = σ0fast + σfast exp[−(t/τfast)β ], 1 < β < 3 (1)

where τfast is the time constant of the process, σ 0fast is theconductivity, when the fast relaxation process is considered tobe finished, and σ fast is the remanent conductivity amplitude.The corresponding resistivity (ρfast = 1/σfast) is shown inFig. 3 for clarity.

The dependences of τfast and β on temperature that wereobtained by fitting the experimental results using (1) are shownin Fig. 5. One can see that at low temperatures (≤120 K), thetime constant is in the order of 220 μs for films with smallerclusters (205 μs for film with larger clusters) and rapidlydecreases with an increase of temperature. The values ofexponent β show similar dependences: for films with smallerclusters these values are also higher at low temperatures (1.55at 120 K) but faster (at lower temperature) approach β = 1value. At T > Tm , the remanent amplitude σ fast is below ourmeasurement accuracy and thus we are not able to measurethis time constant at higher temperatures.

Fig. 4. Conductivity of the fast relaxation process of La-Sr-Mn-O film.Squares: experimental results. Curve: results when fitted to the KAF model.β = 1.55 and τfast = 210 μs.

Fig. 5. Time constant τfast and exponent β dependences on temperature offast conductivity relaxation fitted to the KAF model for three samples withdifferent Tm . Curves: fit to eyes.

These results can be explained as follows: in the paramag-netic state, the magnetization of the film is induced only by theapplication of the external magnetic field. The demagnetizationprocess is determined by the thermal energy and follows intime the magnetic field pulse. In the ferromagnetic state, therelaxation process is determined mostly by the reorientationof the magnetic domains into their equilibrium state. It isknown that for imperfect films, as in our case, these defectsbehave like pinning sites and at first, some reversed spinsor domains appear in the films because of them [5], [9].

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Fig. 6. Conductivity of the slow relaxation process of La-Sr-Mn-O film.Squares: experimental results. Curve: results when fitted to the KWW model.β = 0.79 and τslow = 1.08 ms.

These act as nuclei. Because of their short-range interaction,the adjacent spins reverse more often than others, and magneticdomains grow from these reversed spins. Such magnetiza-tion relaxation is called the Kolmogorov–Avrami model [10],[11] and is originally used by Fatuzzo (F) [12] to interpretthe relaxation processes in ferroelectrics (for more details,see also [5]). However, it is worth mentioning two limitingcases: 1) when nuclei do not grow and relaxation followsthe simple Debye exponent (β = 1) and 2) when domainsgrow extremely fast and relaxation occurs as an compressedexponent ∼exp[−(t/τ)3]. For the intermediate cases, it isproposed that the experimental results be fitted by means of (1)when exponent 1 < β < 3. Our results gave these exponentvalues of 0.95 ≤ β ≤ 1.56 for the measured temperature range250–100 K (Fig. 5). These β values indicate that the nucleationprocess is not fast in these films. The higher τfast and β valuesfor films with smaller clusters at low temperatures could beexplained by the presence of more defects that act as pinningcenters in these films. This is also confirmed by the largerresistivity values. At higher temperatures, the standard Debyerelaxation occurs with a time constant of <60 μs. For filmwith larger clusters, the Tm is higher, therefore, the β showstendency to decrease down to value 1 at higher temperature ifcompare with films with smaller clusters.

B. KWW Relaxation

The slow conductivity relaxation of these La-Sr-Mn-O filmsmeasured while in their ferromagnetic state (T = 100 K) isshown in Fig. 6.

The experimental results are fitted using stretched exponen-tial decay [5]

σ(t) = σ0slow + σslow exp[−((t − t0)/τslow)β ], 0 < β < 1(2)

where t0 is the time instant at which the fast relaxationprocess is considered to be finished and the slow relaxationprocess starts to be analyzed, τ slow is the time constantof the slow process, σ 0slow and σ slow are the conductivitywhen the slow relaxation process is finished and remanent

Fig. 7. Time constant τslow and exponent β dependences on the temperatureof slow conductivity relaxation fitted to the KWW model for three sampleswith different Tm . Curves: fit to eyes.

conductivity amplitude, respectively. The corresponding resis-tivity ρslow = 1/σ slow is shown in Fig. 3.

The results of experiments performed at various tempera-tures using different samples are shown in Fig. 7. One cansee that the time constant of this process at low tempera-tures (100 K) is ∼1.05 ms and decreases with temperature.Because of low measurement accuracy, it is not possible todistinguish different behavior for three investigated films. Theobtained β values of the stretched exponent are in the interval0.65 ≤ β ≤ 0.8 and only slightly decrease with increase oftemperature (Fig. 7, lower part).

The stretched exponential relaxation, first studied byKohlrausch in 1847 [13] and later by Williams and Wattsin 1970 [14], is often used to fit the experimental curves.It is explained as the result of the artificial distribution ofrelaxation times in glassy materials. This model is usuallyknown as KWW relaxation [5]. In such cases, β is used asthe fitting parameter with no microscopic meaning. However,more than decade ago, an axiomatic topological model isproposed [15], [16]. This glassy relaxation is assumed tooccur in an exponentially restricted configuration space thatis drastically different from the conventional free particleconfiguration space. One thus has to assume that the relaxationpaths are obtained by diffusion to relaxation traps or defectsin a configuration space of restricted fractal dimensionality.According to this diffusion-trap model, two special valuesfor the stretching exponent are predicted for the relaxationof microscopically homogeneous glassy systems: β = 3/5for short-range forces and β = 3/7 for long-range forces

2834 IEEE TRANSACTIONS ON PLASMA SCIENCE, VOL. 41, NO. 10, OCTOBER 2013

Fig. 8. Remanent resistivity dependences on magnetic field of slow andfast relaxation processes for three samples with different Tm . Measurementaccuracy 5%.

[15], [16]. Large databases are reviewed that predicted thesemagic values of β, and these are confirmed by investigationsof this process over many decades. Any deviations of β fromthese values are thus assumed to be an indication of the poorquality of the investigated samples and showing a degree ofinhomogeneity. The β values obtained through our investi-gations (0.65 ≤ β ≤ 0.8) indicate that the slow relaxationprocess in the investigated manganite films occurs through onerelaxation channel and is related to short-range interactions inthe defected grain boundaries. The observed (see Fig. 7) slightdecrease of β with temperature showing tendency to approachthe magic value of 0.6 at T ≥ Tm indicates that films inparamagnetic state become more homogeneous.

C. Remanent Resistivity of Fast and Slow Relaxation

It is very important for the development of magnetic fieldsensors that it be cleared up how exactly the remanent resistiv-ity (after the magnetic field pulse is switched off; see Fig. 3)depends on the magnetic field value and ambient temperature.We investigated the dependences of the absolute values as wellas those of the relative parts of the slow and fast componentsin respect to the maximal resistivity change (see Fig. 3).

The absolute values of the remanent resistivity of the slowand fast relaxation processes versus magnetic inductance areshown in Fig. 8. It is obtained that the absolute value of theremanent resistivity of slow relaxation was almost constantin the measured magnetic field range (Fig. 8, upper part).The relative part of it at low fields (2 T) is ∼20% of the

Fig. 9. (a) Magnetic field and (b) temperature dependences of relativeremanent resistivity of slow and fast relaxation processes for three sampleswith different Tm .

whole and decreases with an increase of the magnetic field[see Fig. 9(a)]. Such behavior is promising for the developmentof high magnetic field sensors, since the slow componentbecomes insignificant in high magnetic fields.

The absolute values of the remanent resistivity of the fastcomponent increase with an increase of the magnetic field(see Fig. 8, lower part) and begin to saturate at fields higherthan 10 T. Its relative part amounts to ∼16% of the wholeresistivity change at 4 T and decreases only slightly with anincrease of the magnetic field [Fig. 9(a)]. This component isassumed to be related to the reorientation of the magneticdomains starting with reversed spin nuclei formation at thepinning centers after the magnetic pulse is switched off. Thusit follows that the higher the magnetic field that is applied, thehigher is the magnetization induced by the pulse and the partof it that has to be reoriented after the pulse is switched offbecomes larger. In this case, films with larger crystallites andthus having smaller amounts of defects as pinning centers needto be used in magnetic field sensors to decrease the relativepart of the remanent resistivity. It should be noted that therelative part of the remanent resistivity of fast as well as ofthe slow relaxation components decreases with temperatureand is <2% when approaching Tm [see Fig. 9(b)].

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IV. CONCLUSION

MR relaxation in nanostructured manganite films occurredin three different time scales: ultrafast (<1 μs), fast (∼100 μs),and slow (∼1 ms). The time constants and relative partsof the remanent resistivity of the slow and fast componentsdecreased rapidly with an increase of temperature and arenegligible in the paramagnetic state of the films. The relativepart of the fast component was only slightly dependent on themagnetic field and can be decreased by using films with largercrystallites. For the measurement of high-pulsed magneticfields with durations longer than several milliseconds, thiscomponent played an insignificant role. The absolute value ofthe remanent resistivity of the slow component was constantand thus the relative part of it decreased with an increase of themagnetic field. It could be <5% when approaching megagauss.

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Nerija Žurauskiene (M’10) received the Ph.D. degree in physics from theSemiconductor Physics Institute, Vilnius, Lithuania, in 1996.

She is currently a Senior Research Scientist with the SemiconductorPhysics Institute, Center for Physical Sciences and Technology, Vilnius,and a Professor with Vilnius Gediminas Technical University, Vilnius. Sheis the co-author of more than 100 scientific papers. Her current researchinterests include investigation of short high power electric and magneticpulses influence on low dimensional solid-state materials, investigation ofoptical properties of semiconductor quantum dots, and design of magneticfield sensors and protectors against EMP.

Dr. Žurauskiene received the Lithuanian National Award in Science in2000.

Saulius Balevicius (SM’01) received the Ph.D. degree in physics from theVilnius University, Vilnius, Lithuania, in 1980, and the Habilitation Doctordegree in physics from the Semiconductor Physics Institute, Vilnius, in 2002.

He is currently the Head of the Department of Material Sciences andElectrical Engineering, Semiconductor Physics Institute, Center for PhysicalSciences and Technology, Vilnius, and a Professor with the Vilnius GediminasTechnical University, Vilnius. He is the author or co-author of more than 100scientific papers and owner of 24 inventions. His current research interestsinclude the influence of high-power electric, magnetic, and light and shockwave pulses on solid-state materials.

Dr. Balevicius received the Lithuanian National Award in Science in 2003.

Dainius Pavilonis received the M.S. degree in physics from Vilnius Univer-sity, Vilnius, Lithuania, in 2012. He is currently pursuing the Ph.D. degreewith the Semiconductor Physics Institute, Center for Physical Sciences andTechnology, Vilnius.

His current research interests include the investigation of high pulsedmagnetic fields influence on perovskite manganite thin films.

Voitech Stankevic received the Ph.D. degree in physics from the Crystallog-raphy Institute, Moscow, Russia, in 1986.

He is currently a Senior Research Associate with the SemiconductorPhysics Institute, Center for Physical Sciences and Technology, Vilnius,Lithuania, and an Associate Professor with Vilnius Gediminas TechnicalUniversity, Vilnius. He is the co-author of more than 40 scientific papers. Hiscurrent research interests include material engineering, semiconductor pres-sure sensors technology, design of various converters, manganites technologyand research, and development of magnetic field sensors.

Skirmantas Keršulis received the Ph.D. degree in physics from VilniusGediminas Technical University, Vilnius, Lithuania, in 2010.

He is currently a Junior Researcher with the Semiconductor PhysicsInstitute, Center for Physical Sciences and Technology, Vilnius. He is theco-author of ten scientific papers. His current research interests include theinvestigation of short high power electric and magnetic pulses influence onsolid-state materials.

Jurij Novickij received the Ph.D. degree in electrical engineering andelectronics from Vilnius Gediminas Technical University, Vilnius, Lithuania,in 2000.

He is currently a Senior Research Scientist, the Head of High MagneticField Laboratory and a Professor with Vilnius Gediminas Technical University.He is the co-author of more than 50 scientific papers. His current researchinterests include the generation and application of high magnetic and electricalfields in applied physics, material science, biomedicine and industry.