Selected size effects in magnetic nanocrystalline systems and thin layers
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1 Selected size effects in magnetic nanocrystalline systems and thin layers Habilitation Thesis Tadeusz Szumiata Laboratory of Magnetic Materials Department of Physics Faculty of Mechanics Technical University of Radom Krasickiego 54, Radom, Poland
2 My great thanks to Dr. hab. Katarzyna Brzózka, Prof. Wiesław Wasilewski, M.Sc. Michał Gawroński, M.Sc. ing. Bogumił Górka and Dr. Kazimierz Hibner my colleagues from Department of Physics at Technical University of Radom for help, common hard work in Mössbauer Laboratory, kindness and longtime friendship, to Prof. Pavol Sovák, Prof. Peter Kollár and all my collaborators from Faculty of Science in P.J. Ńafarik University in Końice - for great friendliness and cooperation on magnetic nanocrystalline alloys, to Prof. Mike Gibbs, Dr. Nicola Morley, Dr. Athar Javed and all my friends from Department of Materials Science and Engineering in University of Sheffield (U.K.) for very effective cooperation and help in the field of magnetic thin films as well as unusual hospitality during my scholarship staying in Sheffield, to Dr. Ryszard Żuberek and Prof. Anna Ślawska-Waniewska from Institute of Physics of Polish Academy of Sciences in Warsaw for fruitful collaboration on magnetostriction of nanocrystalline alloys and for longtime friendship, to Prof. Tadeusz Kulik - Vice-Rector for Scientific Research of Warsaw University of Technology for great kindness and help in fabrication and structural characterisation of nanocrystalline magnetic materials, to M.Sc. Józef Balcerski from Solid State Physics Department in Faculty of Physics and Applied Computer Science in University of Łódź for thin films fabrication, to my Family for great tolerance and patience. 2
3 The habilitation is based on12 articles [1] T. Szumiata, M. Gawroński, B. Górka, K. Brzózka, J. S. Blázquez-Gámez, T. Kulik, R. Żuberek, A. Ślawska-Waniewska, "Hyperfine fields and magnetoelastic surface effects in Fe 72 Cu 1.5 Nb 4 Si 13.5 B 9 nanocrystalline alloy", Nukleonika 48 Suppl. 1 (2003) pp. S85-S88. [2] T. Szumiata, K. Brzózka, M. Gawroński, B. Górka, J. S. Blázquez-Gámez, T. Kulik, R. Żuberek, A. Ślawska-Waniewska, "Mössbauer and magnetoelastic investigations of the surface effects in Fe 72 Cu 1.5 Nb 4 Si 13.5 B 9 nanocrystalline alloy", Journal of Magnetism and Magnetic Materials (2004) pp [3] K. Brzózka, T. Szumiata, M. Gawroński, B. Górka, P. Kollár, P. Petrovič, "Mössbauer spectroscopy temperature investigations of Fe-Si-Cu-Nb-B powder", Czechoslovak Journal of Physics 54 Suppl. D (2004) pp. D193-D196. [4] T. Szumiata, B. Górka, A. Zorkovská, P. Sovák, "Structure and hyperfine interactions in Al-doped FINEMET", Journal of Magnetism and Magnetic Materials 288 (2005) pp / 295 (2005) pp [5] A. Javed, T. Szumiata, N.A. Morley, M.R.J. Gibbs, "An investigation of the effect of structural order on magnetostriction and magnetic behavior of Fe-Ga alloy thin films", Acta Materialia 58 (2010) pp IMPACT FACTOR:
4 [6] T. Szumiata, K. Brzózka, M. Gawroński, B. Górka, A. Javed, N. A. Morley, M. R. J. Gibbs, "Structural and magnetic ordering in Fe-Ga thin films examined by Mössbauer spectrometry", Acta Physica Polonica A 119 (2011) pp [7] K. Brzózka, T. Szumiata, P.Sovák, B.Górka, K.Hibner, J. Balcerski, "Finemet thin films substituted by chromium CEMS and MOKE study", Acta Physica Polonica A 118 (2010) pp [8] T. Szumiata, M. Gzik-Szumiata, K. Brzózka, "Modelling of thermomagnetic curves obtained with Mössbauer spectromery for two-phase nanocrystalline alloys", Materials Science - Poland 25 (2007) pp [9] T. Szumiata, M. Gzik-Szumiata, K. Brzózka, M. Gawroński, B. Górka, "Modeling of magnetic hyperfine field distribution for spherical nanoparticles of bcc structure", Acta Physica Polonica A 113 (2008) pp [10] T. Szumiata, M. Gzik-Szumiata, K. Brzózka, "Pseudodipolar model of surface magneto-striction for thin layers with roughness", Materials Science - Poland 26 (2008) [11] T. Szumiata, M. Gzik-Szumiata, K. Brzózka, "Electrical resistivity dependence on surface roughness geometry in thin films", Acta Physicae Superficierum 11 (2009) pp [12] T. Szumiata, M. Gzik-Szumiata, "Model of anisotropic electrical resistivity in rough thin films", Acta Physica Polonica A, 118 (2010) pp
5 Criteria (P. J. Šafárik University in Košice) Required Fulfilled 1. Educational activity: - Period [years of employment] Handbooks and scripts Publications: - In total From Current Content data base Citations: - In total (excluding autocitations) WoS and SCOPUS citations Grants and scientific projects 2 4 5
6 Outline Motivation General thesis and questions Experimental research on nanocrystalline alloys Experimental research on thin layers Theoretical models General conclusions 6
7 Motivation Inspired by Feynman: There is Plenty of Room at the Bottom Richard Feynman, December 29th 1959, annual meeting of the American Physical Society at the California Institute of Technology (Caltech) Two-phase nanocrystalline alloys [e.g. FINEMET of Fe 73.5 Nb 3 Cu 1 Si 13.5 B 9 composition originally proposed by Yoshisawa (1988) and NANOPERM Fe(Zr,Nb)B(Cu,Y,Mo)] are known for very high effective permeability, high saturation magnetization, small magnetostriction and coercivity. Thou nanocrystalline materials have already found wide applications (e.g. as excellent lossless transformer cores, in microwaves inductors) the physics of them is not entirely understood. Some questions are still open especially connected with size effects resulting from the presence of nanograins and their surface. The interface region between grains and amorphous matrix is very difficult to evidence with X-ray diffraction. Mössbauer spectroscopy seems to be a very helpful technique for this purpose. Thin films of magnetostrictive materials with low saturation field (H s ), low coercivity (H c ) and significant saturation magnetostriction constant ( s ) have applications in magnetic microelectromechanical systems (MagMEMS) and possibly in spintronics. Low-cost Fe-Ga alloys (Galfenols) are of interest due to their superior magnetic and mechanical properties over other magnetostrictive materials (e.g. Terfenol-D and shape memory alloys). On the other hand, magnetically soft thin films of FINEMET substituted by Cr seem to be very important for applicational point of view e.g. they can be used for fabrication of magnetic thin film inductors in high-frequency technique. Present work is focused mainly on thickness dependent effects (structural variations, internal stress evolution, spin texture and magnetic anisotropy of the films). 7
8 General theses and questions 1. Is it possible to evidence with Mössbauer measurements grains interface (surface) contribution in the case of nanocrystalline alloys possessing nanocrystallites of more complex structure (like in FINEMET) than in the NANOPERM? What is a thickness of the interface region? 2. What kind of size effects are the result of milling process of amorphous FINEMET ribbons studied by means of Mössbauer spectroscopy? 3. Thermomagnetic curves peculiarities of nanocrystalline grains especially slope drop beyond a Curie point of amorphous matrix (observed effectively with Mössbauer spectroscopy) may be regarded as universal feature for nanocrystalline alloys. 4. Fe-Ga alloys in 2D form of thin layers possibly have greater magnetostriction than in the case of bulk due to reduction of DO 3 and L1 2 structural ordering and may be a good candidates for Mag-MEMS applications. Mössbauer (CEMS) experiments may detect some structural and magnetic size effects (e.g. thickness-dependent spine texture, magnetic anisotropy and internal stress) in Fe-Ga thin films. 8
9 5. Thin films of chromium-doped FINEMET are expected to be the objects revealing complex magnetic anisotropy due to the influence of the substrate and internal stress. Magnetooptical (MOKE) experiments combined with Mössbauer (CEMS) measurements may be very helpful in detecting these phenomena, typical for 2D thin layered systems. 6. Superferromagnetic intergrain interactions are presumably crucial for proper theoretical modelling of nanocrystalline grains thermomagnetic behaviour in the vicinity of Curie point of amorphous matrix in two-phase nanocrystalline alloys. Phenomenological description in the case of these complex systems possibly demands an effective exchange integral for nanocrystallites depending on mean spin value of the amorphous phase. 7. Is it possible to predict theoretically a form and temperature dependence of hyperfine field distribution of spherical nanoparticles and nanocrystallites basing on hyperfine parameters values for thin films surface known from Mössbauer (CEMS) experiments? 8. The surface roughness should be a very important factor influencing the effective magnetostriction of thin films. Both electronic and dipolar contribution to surface magnetostriction should be affected by roughness. 9. What kind of size effects in the electrical conductivity of thin monolayers are caused by surface roughness? Is it possible to predict CIP CPP (current-in-the-plain currentperpendicular-to-the-plain) anisotropy just by static averaging of mean free path over the whole structure of rough film? 9
10 Experimental research on nanocrystalline alloys Surface effects in nanograins [1] 10
11 [2] 11
12 Fe-Si nanograins in FINEMET - complicated multisextet Mössbauer spectrum Ranges of HFD for grains and matrix are everlaped at room temperature These two factors make difficult to find traces of the interface phase. Idea: to elevate temperatures (but T < T C am ) Result: HFD --> low HFD(am) + high HFD(if) Mössbauer measurements carried out at elevated temperature confirmed a presence of structural interface effects Estimated thickness of interface: h i 0.5 nm (i.e. about two atomic layers). Additional confirmation - Magnetostriction 12
13 Effective magnetostriction constant Surface term 13
14 Experimental research on nanocrystalline alloys Size effects in powdered aloys [3] 14
15 Ball-milling of as-quenched (amorphouse) FINEMET ribbons In one material - - two interesting magnetic features connected with size effects of the grains: Long milling: significant dispersion of grains sizes Superparamagnetism (for several nm grains) -nonmagnetic doublet even at liquid nitrogen temperatures (blocking temperature is lower) After milling: partial nanocrystallisation of amorphouse FINEMET ribbons powder Superferromagnetism (for larger grains containing many nanocrystallites) superferromagnetic interactions between nanocrystallites via amorphouse matrix are weakened due to finite sizes of powder grains (in comparison with alloys of the form of bulk ribbons) magnetism of nanocrystallites drops beyond Curie temperature of 15 amorphouse matrix
16 Experimental research on nanocrystalline alloys Thermomagnetic curves peculiarities [4] 16
17 17
18 Size effect: superferromagnetism of nanocrystallites in two phase magnetic material 18
19 Constant thickness Various Ga content Experimental research on Fe-Ga thin layers Structural ordering and magnetostriction [5] 19
20 Magnetostriction optimization (no DO 3 nor L1 2 structure!!!) Mössbauer results will be presented in details for another series of samples. 20
21 Various thickness Constant Ga content Experimental research on Fe-Ga thin layers Structural and magnetic size effects [6] 21
22 CEMS - Spectra CEMS - HFD No DO 3 nor L1 2 structure!!! Domination of BCC disordered A2 phase. DO 3 (Fe 3 Ga) L1 2 (Fe 3 Ga) 22
23 Size effects: Nonmonotonic dependence of lattice constant on film thickness anomaly for Nonmonotonic dependence of hyperfine parameters on film thickness t = 40 nm [ Interpretation internal stress evolution during growth process] Spin texture reveals a transition from the in-plane to out-of-the-plane configuration with increasing thickness (monotonic dependence of angle) [ Interpretation perpendicular magnetocrystalline anisotropy rise (in relation to dipolar one )] 23
24 [7] 24
25 Y X
26 26
27 [8] 27
28 28
29 [9] 29
30 30
31 [10] 31
32 32
33 Pseudodipolar model electronic contribution (exchange interactions, magnetocrystalline anisotropy) Dipolar magnetic interactions 33
34 [11] 34
35 35
36 [12] 36
37 Present results concerning thickness dependence of CIP resistivity for smooth films are very close to those in former work [4] obtained by static averaging of isotropic MFP. However in the case of rough surfaces the present model predicts higher CIP resistivity by about 20% for t/l 0 = 0.5 and by about 40% for t/l 0 = It could be explained by the fact that new model based on dynamic simulation considers in the natural way a trapping of electrons by surface roughness. 37
38 General Conclusions 1. Mössbauer measurements at elevated temperatures confirm a presence of structural interface effects in FINEMET-type Fe 72 Cu 1.5 Nb 4 Si 13.5 B 9 nanocrystalline alloy that was additionally supported by magnetostrictive investigations. Both a thickness of the interface region and surface magnetostriction constant have been estimated. Size effects in nanocrystalline materials seems to be important not only for alloys of simple structured grains (e.g. NANOPERM) but they are universal feature for this kind of materials. Mössbauer spectrometry not only sees the interface region (HREM would be better) but points to the significant changes in physical properties of the inteface (via hyperfine parameters). 2. FINEMET powder studies by means of Mössbauer spectroscopy show that milling process is responsible for several kinds of size effects in magnetic of nanocrystalline alloys e.g. nanocrystallisation, superparamagnetism, weakened superferromagnetism and grain boundaries influence. 3. The peculiarities of thermomagnetic curves of nanocrystalline grains (slope drop) beyond a Curie point of amorphous matrix are universal feature for nanocrystalline alloys. It has been proved with Mössbauer spectroscopy that addition of Al to FINEMET alloy does not change the character of thermomagnetic behaviour (thou it reduces Curie temperatures). 4. Two-dimensional character of growth process of Fe-Ga thin films (with co-sputtering and evaporation technique) effectively reduces a tendency to DO 3 and L1 2 structural ordering, what has been clearly confirmed in XRD and CEMS experiments. This result foster a fabrication of high-magnetostrictive films based on Fe-Ga alloy for Mag-MEMS applications. Other interesting size effects observed in the investigated films are: thickness evolution of spin texture, perpendicular magnetocrystalline anisotropy, internal stress as well as possible influence of surface roughness on effective magnetostriction constant. 38
39 5. Chromium-doped FINEMET thin films reveal several 2D-type magnetic features, like in-plain magnetization alignment and in-plain magnetic anisotropy (i.e. angular dependence of the coercivity) evidenced by magnetooptical (MOKE) and Mössbauer (CEMS) measurements. Since FINEMET(Cr) layers are distinguished by relatively small coercivity, they are good candidates for base material for new generation microwaves inductors. 6. Proposed theoretical model of thermomagnetic behaviour of nanocrystalline grains beyond a Curie point of amorphous matrix in two-phase nanocrystalline alloys fits well experimental data from Mössbauer spectrometry. Surface effects and weakenning of superferromagnetic intergrain interactions has been simulated with effective exchange integral for one phase depending on mean spin value of the other phase. 7. Model, based on MFA calculations and utilizing hyperfine parameters of thin magnetic layers surface, predicts a hyperfine field distribution of spherical nanoparticles (or nanocrystallites) surface at given temperature however realistic simulation of all possible atomic environments and lattice distortions at spherical surface would be a very complex task. 8. Theoretical considerations convince that electronic contribution to the surface magnetostriction of bcc Fe monocrystalline films increases with increasing surface roughness and prove that magnetic dipolar contribution is also not negligible. 9. Developed theory of electrical transport in thin monolayers effectively predicts several size effects, like rapid increase of electrical resistivity for very thin films (compared to mean free path) and its CIP CPP anisotropy caused by rough surface. In order to reproduce this anisotropy, dynamic simulations are necessary considering electrons trapping by roughness. 39
40 Answers to the questions of Oponents 40
41 Prof. 41
42 NO YES BOTH 42
43 Volumetric fraction of grains determined from the Mössbauer spectra should be a sum of grain core contribution and surface-interface contribution. When spectra are too complex it is extremely difficult to subtract surface-interface contribution from amorphous matrix contribution. It is a source of uncertainties. 43
44 The information in the text possesses only a technical (not scientific) meaning. It has been just underlined, that genetic algorithm was utilized, what prevent wandering around local minimum of 2 function. 44
45 Prof. 45
46 Mössbauer spectra are too complex No possibility of high temperature CEMS EM nor AFM pictures not available yet (grain size) Question of grain interface and surface interface 46
47 Y X
48 Present model: effective exchange integral Future: individual spins of 2D model 48
49 49
50 Direct techniques Indirect techniques question of elastic <-- constants of the substrate 50
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