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Magnetic Properties of Nanostructured Thin Films of Transition Metal Obtained by Low Energy Cluster Beam Deposition V

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Magnetic Properties of Nanostructured Thin Films of Transition Metal Obtained by Low Energy Cluster Beam Deposition V Magnetic properties of nanostructured thin films of transition metal obtained by low energy cluster beam deposition V. Dupuis, J. P. Perez, J. Tuaillon, Vincent Paillard, P. Mélinon, A. Perez, B. Barbara, L. Thomas, S. Fayeulle, J. M. Gay To cite this version: V. Dupuis, J. P. Perez, J. Tuaillon, Vincent Paillard, P. Mélinon, et al.. Magnetic properties of nanostructured thin films of transition metal obtained by low energy cluster beam deposition. Journal of Applied Physics, American Institute of Physics, 1994, 76 (10), pp.6676 - 6678. 10.1063/1.358165. hal-01660437 HAL Id: hal-01660437 https://hal.archives-ouvertes.fr/hal-01660437 Submitted on 10 Dec 2017 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Magnetic properties of nanostructured thin films of transition metal obtained by low energy cluster beam deposition V. Dupuis, J. P. Perez, J. Tuaillon, V. Paillard, P. Mélinon et al. Citation: J. Appl. Phys. 76, 6676 (1994); doi: 10.1063/1.358165 View online: http://dx.doi.org/10.1063/1.358165 View Table of Contents: http://jap.aip.org/resource/1/JAPIAU/v76/i10 Published by the American Institute of Physics. Additional information on J. Appl. Phys. Journal Homepage: http://jap.aip.org/ Journal Information: http://jap.aip.org/about/about_the_journal Top downloads: http://jap.aip.org/features/most_downloaded Information for Authors: http://jap.aip.org/authors Downloaded 27 Apr 2013 to 130.113.111.210. This article is copyrighted as indicated in the abstract. Reuse of AIP content is subject to the terms at: http://jap.aip.org/about/rights_and_permissions Magnetic properties of nanostructured thin films of transition metal obtained by low energy cluster beam deposition V. Dupuis, J. P. Perez, J. Tuaillon, V. Paillard, P. MGlinon, and A. Perez Dgpartement de Physique des Matiriaux, Universitg Lyon, 1-69622 Weurbanne C&dex, France B. Barbara and L. Thomas Laboratoire de Magndtisme Louis Nt?el, CNRS BP166X-38042 Grenoble Cgdex, France S. Fayeulle Dgpartement Mat&aux Mkanique Physique, Ecole Centrale de Lyon, BP 16369131 Ecu&, France J. M. Gay CRh4C2, Campus de Luminy, CNRS-13397, Marseille Ct?dex 13, France Clustersof iron, cobalt, andnickel areproduced in a laservaporization source. The size distributions of the incident clusters are checkedby time-of-flight mass spectrometrybefore deposition at low energy.Studying the near threshold photoionization,Co, and Ni, clusters exhibit an icosahedral structure while for iron, no clear structure emerges.Neutral clusters were depositedon different substratesat room temperaturewith thicknessesup to 100 nm in view to determinetheir structure and magnetic properties.A limited coalescenceof the clusters is observedfrom high-resolution transmission electron microscopy. No icosahedron has been observed but cuboctahedronand interfacetwins betweenadjacent particles have been clearly identified in Ni films. Grazingincidence x-ray diffraction experimentsreveal a classicalphase with grain size around6 and 4 mn for Fe and Ni fYms, respectivelybut an anomalousfee phasefor Co fdms and a very low grain size of 2 nm. The density of films determinedby x-ray reflectivity was estimatedto representonly 60%-65% of the bulk density.Magnetic behaviors studied by ferromagneticresonance and SQUID magnetization measurementshave been interpreted using the correlated spin glass model. Miissbauer spectra performed on Fe films at zero field revealed the presenceof 20% of iron in the form of thin nonmagneticoxide skin surroundingFe grains which allow to fmd 2.2 ,LLBper magneticiron atom in agreementwith macroscopic magnetic measurements.Nevertheless we found an anomalous reducedatomic moment for Ni film. INTRODUCTION Our challengein depositingtransition metal clustersis to synthesizenew phaseswhere the anomalouscrystallographic Recently,magnetic properties such as exchangecoupling structures of free clusters would be kept and to study the or giant magnetoresistancemainly observedin metallic mul- specific magnetic behavior of these weakly correlated enti- tilayers have been detectedin other nanostructuredsystems. ties on a substrate.Once more, we show that our technique For example,Berkowitz et a1.l and Xiao et al.’ observedgi- leads to a random compact cluster stacking (RCCS).3Thus ant magnetoresistancesin ultrafine Co-rich precipitate par- magnetic results could be interpretedby random anisotropy ticles in a Cu-rich matrix. These sampleswere preparedby model with a scale law and in terms of localization of spin coevaporationtaking advantageof the low solubility of Cu in waves. Co. However, though this techniqueis limited to nonmiscible components,the adjustablecluster diameteris a new param- eter in addition to the distancebetween particles as in thin EXPERIMENT film layers. Thus, studies on clusters and cluster assembled Our cluster source is based on the technique of laser materialsare of increasinginterest. vaporization.3-5Roughly, a plasma is created in a vacuum The laser vaporization source of the laboratory3allows cavity by Nd-YAG laser light. Synchronizedwith the laser, a the obtentionof an intensecluster beamof any size distribu- high pressure(5 bars) helium pulse, injected in the cavity by tion (from few to a thousandatoms per cluster) and the syn- a nozzle, thermalizesthe plasma and cluster growth occurs. thesis of cluster assembledmaterials, even of the most re- The nascentclusters are then rapidly quenchedduring the fractory and of the most complex ones. The cluster size following isentropic expansioninto vacuum (lo-’ Torr). distribution is checked by time-of-flight mass spectrometry Cluster size distributions are analyzedin a time-of-flight before deposition. Our source producing cold clusters with mass spectrometer.Studying the near threshold photoioniza- low kinetic energy,incident clusters do not fragment on the tion (performedwith a frequency-doubledtunable dye laser substrateand may conserve their intrinsic structures.Thus pumpedby a XeCl excimer laser), mass spectraof Co, and we succeeded in the stabilization of very small size Ni, clusters exhibit oscillations and a series of magic num- fullerenes (C&L&J, never previously observedexperimen- bers in=13,55,147,309,561,...) corresponding to an tally. We clearly evidenced that deposited carbon clusters icosahedralor cuboctahedralatomic shell structurein the ob- presentedthe in flight-clusters fingerprint? tained massrange (50-800 atomsper cluster). A finer analy- 6676 J. Appt. Phys. 76 (lo), 15 November 1994 0021-8979/94/76(10)/6676/3/$6.00 0 1994 American Institute of Physics Downloaded 27 Apr 2013 to 130.113.111.210. This article is copyrighted as indicated in the abstract. Reuse of AIP content is subject to the terms at: http://jap.aip.org/about/rights_and_permissions sis allows us to conclude for the icosahedralstructnre.6 For iron clusters, the results are not so simple, indicating a com- r/ petition between different regimes.6 --, I,, I...I, .I Then, free neutral clusters are deposited with a kinetic energy in the lo-20 eV range on different substratesat room temperaturewith thicknessesup to 100 nm in view to deter- mine their structure and magnetic properties. SAMPLE CHARACTERIZATION The typical size of supported clusters obtained from high-resolution transmissionelectron microscopy (HRTEZM) was about 2-6 nm for an initial size distribution centered around 150 atoms for Fe and 300 atoms for Co and Ni clus- ters, respectively. No icosahedronwas observedbut cuboc- tahedra and interface twins between adjacent particles was clearly identified in Ni films. Quasisphericalgrain morphol- ogy existed in Fe film which could correspond to a bee rhombic dodecahedron Cl101 according to the Wulff’s theorem.7 Grazing incidence x-ray diffraction (GIXD) ex- periments exhibit a classicalbee phasefor Fe fI.lms but a fee phasefor both Co and Ni with a grain size extractedfrom the -12 -8 -4 0 4 8 12 peak width of about 6, 4, and 1.5 nm, respectively,in agree- VELOCITY mm/s ment with electronic diffractions and TEM observations.The classical structure of cobalt being hcp, the fee phase ob- FIG. 1. Mkbauer spectra obtained on a Fe,,, film at 300 K. served in Co films might be related to the icosahedralstrut- ture of the incident cluster beam. In fact, the icosahedronis expected to be the precursor of the fee crystal. The small The macroscopic magnetic behavior of our films has grain size and the reminiscence of a free cluster structure been studiedusing ferromagneticresonance (FMR) and mag- confirm the limited coalescenceprocess due to a weak diffu- netization measurements(SQUID). FMR curves roughly tra- sion of metallic clusters on the substrateeven at room tem- duced a thin film behaviorrl but revealed several resonance perature. magnetic fields due to anchorageof spin waves at the surface Rutherford backscattering spectroscopy showed that (when the applied field is perpendicularto the surface of the theseporous films are composedof 2070~30%of oxygen for film). The coercive field at 300 K is about 100 Oe for cobalt, 70%-80% of metals. The density of the films, determinedby
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