Magnetic Properties of Electrodeposited Nanocrystalline Ni-Fe alloys
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1 Magnetic Properties of Electrodeposited Nanocrystalline Ni-Fe alloys Minghe Wang Supervisor: Dr. Marek Niewczas 701 Graduate Seminar 18 th September, 2012
2 Origin of the magnetism Only atoms with partially filled electron shells have a magnetic moment. Schematics of the electron s motion around the nucleus Ferromagnetic materials Refrigerator magnet used to hold notes on a refrigerator door 2
3 Soft magnetic materials Large hysteresis loss Low permeability Large Coercivity values Low hysteresis loss High permeability Small Coercivity values 3
4 Nanocrystalline soft magnetic materials Read-write head 28 Ni Low λs Transformer cores 26 Fe Candidates 27 Co Magnetic shielding 4
5 Magnetocrystalline Anisotropy How do magnetic materials react to magnetic field? BCC-Fe FCC-Ni 5
6 Random Anisotropy Model D > L ex the magnetization will follow the individual easy magnetic directions of the structural units. D < L ex the effective anisotropy for the magnetic behavior will be an average over several structural units and, thus, be reduced in magnitude. D L ex = K = K A K 1 N = K 1 D L ex G. Herzer., Scripta Met. 33, Exchange stiffness Effective magnetocrystalline anisotropy 3/ 2 K 1 Exchange interaction averages over anisotropy of individual grains 6 L ex
7 Objectives Develop a better understanding of the relationship between composition, microstructure and the magnetic properties of NiFe nanocrystalline materials between 2K and 298K. Materials Nanocrystalline Ni - x% Fe alloys (x=24,32,43,53,59) samples produced by electrodeposition from Integran Technologies Inc. were in the form of foils (~ 50 µm). Circular disk samples with 3 mm in diameter were cut from the foils and were used for the characterization. Outline Structure and Texture characterization Magnetic property characterization Conclusions 7
8 Part 1: Texture and Structure 2D XRD instrument Materials: nc-ni-fe alloys provided by Integran Technologies Inc. ~50um 8
9 TEM characterization Grain size ~10nm --- G.A. Cingara Ni-32wt.% Fe 40 Ni-24wt.% Fe Grain size(nm) Grain size calculated from XRD Ni-43wt.% Fe Ni-53wt.% Fe Fe content (wt.%) Ni-59wt.% Fe
10 Structure determination For alloy with an iron content of 59 percent, a mixed BCC and FCC structure was obtained. All the other alloys with different iron content as expected are composed entirely of γ phase FCC structure. (111) BCC FCC (200) BCC (220) Intensity(a.u.) FCC + BCC Fe content (wt.%) Theta(Degree) The Fe-Ni phase diagram from literature (G. Cacciamani, Intermetallics, Vol. 18, No. 6, 2010, pp ) X-ray diffraction pattern of nanocrystalline Ni-x wt. % Fe alloys (x=24,32,43,53,59) 10
11 Structure determination Solid solution structure of Fe in Ni is confirmed. The lattice parameters increased linearly with increasing the iron content of FCC Ni-Fe alloys, and reached a maximum value at Ni- 53wt. % Fe Lattice parameter a (Å) Ni atoms Fe atoms Schematic representation of solid solution of Fe in Ni Fe CONTENT(wt.%) Lattice parameter as a function of the Fe content in electrodeposited Ni-Fe alloys 11
12 Texture analysis Major component of the <100> fibre texture, and some contribution of the <111> and <110> component. Ni-24wt.%Fe Ni-32wt.%Fe Ni-43wt.%Fe Ni-53wt.%Fe Ni-59wt.%Fe Calculated pole figures of Ni-Fe alloys with different Fe content 12
13 Texture analysis The maximum value of the random orientation fraction was obtained for the Ni-43wt.% Fe nanocrystalline alloy. Spread angle 10 degree Volume fraction (%) (100) (111) Fe CONTENT(wt.%) Random orientation fraction(%) Fe CONTENT (wt.%) Calculated Fe content dependence of volume fraction (a) <100> and <111> fibre, (b) random 13
14 Part 2: Magnetic property characterization (PPMS & SQUID) Out of plane ~50um In plane 14
15 H, T=2K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe H, T=298K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe H, T=2K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe µ 0 H (Telsa) µ H (Tesla) H, T=298K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe µ 0 H (Tesla) µ H (Tesla) 15
16 Magnetic properties H, T=2K H, T=298K H, T=2K H, T=298K D 6 1/D Ms (emu/g) Hc(Oe) H, T=2K H, T=298K H, T=2K H, T=298K Fe content Coercivity as function of grain size for numerous materials After G. Herzer, Nanocrystalline soft magnetic alloys. In: Buschow KHJ, editor. Handbook of Magnetic Materials, vol. 10. Elsevier Science B.V., p.415 (1997) In plane and out of plane saturation magnetization and coercivity as a function of Fe content at 2K and 298K 16
17 Law of Approach To Saturation structural defects and non-magnetic inclusions uniform magnetocrystalline anisotropy high field susceptibility H, T=2K µ 0 H (Telsa) e d c b a H, T=298K µ 0 H (Tesla) Open square: experimental curve (dots) Straight lines: best fit Ni-xwt.%Fe a)x=24,b)x=32,c)x=43,d)x=53,e)x=59 17 e d c b a
18 Effective Magnetocrystalline Anisotropy K eff = = K M s 105 a 8 The values of Ms and a2 obtained from fitting the experimental data 2 Sample Ni- 24wt.%Fe Ni- 32wt.%Fe Ni- 43wt.%Fe Ni- 53wt.%Fe Ni- 59wt.%Fe Ms (emu/g) T=2K a 2 (10 4 Oe) 2 K eff (erg/cm 3 ) Ms (emu/g) T=298K a 2 (10 4 Oe) 2 K eff (erg/cm 3 ) *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E *E5 18
19 Effective Magnetocrystalline Anisotropy The maximum value K eff was obtained with Ni-43wt.%Fe alloy Keff(10 5 erg/cm 3 ) T=2K T=298K Random orientation fraction(%) Fe CONTENT(wt.%) The effective magnetocrystalline anisotropy as a function of Fe content Fe CONTENT (wt.%) Calculated Fe content dependence of random orientation fraction 19
20 Exchange Length Exchange length decreases with increasing Fe content L ex > D Samples Exchange length L ex (nm) T=2K T=298K Grain size D (nm) Ni-24wt.%Fe Ni-32wt.%Fe Ni-43wt.%Fe Ni-53wt.%Fe Ni-59wt.%Fe
21 Inverted hysteresis loops Regular B H, T=2K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe -150 µ 0 H (Telsa) H, T=2K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe µ 0 H (Telsa) µ 0 H (Tesla) µ 0 H (Tesla) H, T=298K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe -150 µ 0 H (Tesla) H, T=298K Ni-24 % Fe Ni-32 % Fe Ni-43 % Fe Ni-53 % Fe Ni-59 % Fe µ 0 H (Tesla) µ 0 H (Tesla) µ 0 H (Tesla) Mr (emu/g) Inverted H, T=2K H, T=298K H, T=2K H, T=298K B Fe (wt.%) H H In plane and out of plane remance as a function of Fe content at 2K and 298K Inverted parallel and perpendicular hysteresis loops (Inset) An enlarged view of the same curves. 21
22 Inverted hysteresis loops Two-phase model: The crystalline component and the boundary component featured antiferromagnetic exchange interaction. Schematic representation of a nanocrystalline material :. Black: atoms within the crystallite lattice, White: atoms at the grain boundaries. (R. BIRRINGER, Materials Science and Engineering, A117(1989) ) The exchange interaction between the oxide layer on the surface and the NiFe nanocrystalline alloy. 22
23 Conclusions The nanocrystalline Ni-xwt.%Fe alloys (x = 24,32,43,53) are comprised exclusively of the γ-fcc phase, whereas the coexistence of Ni-rich FCC and Fe-rich BCC phases are clearly observed from the X-ray diffraction patterns of Ni-59wt.%Fe alloy. The lattice parameter calculations have shown that the addition of Fe to Ni expanded the lattices. all the samples have fibre texture with strong <100> component and some contribution of the <111> component. With increasing Fe content, the Hc decreased until 43wt.%Fe. (The lowest Hc is around 6 Oe.) whereas the Ms increased monotonously and approached the highest value at 170 emu/g (with 59 wt.%fe), remnant magnetization are negative for all samples. The highest value of K eff is obtained for 43 wt. % Fe samples. The ferromagnetic exchange length decreases with increasing Fe content. the Random Anisotropy Model is suitable to describe properties of nanocrystalline Ni-Fe alloys. 23
24 Acknowledgement Dr. Marek Niewczas Integran Technologies Inc. for electrodeposited Ni-Fe alloys. Prof. Uwe Erb, University of Toronto Dr. Gordana Cingara and Dr. Qiuping Bian Financial support Ontario Research Fund in U of T/McMaster/ Integran Technologies Research Project on Electrodeposited Soft Magnetic Nanomaterials 24
25
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