Institute of Deformation and Fracture DF Materials in PM Materials Fe Academia Cr Center, Stara Lest Research Ste sencen ii Soft magnetic composite material base on ferromagnetic powders and ferrites Magdaléna Stretkova, Hynek Hadraba, Radovan Bure’, Pavla Roupcova, Vladimir Girman Institute of Materials Research, Slovak Academy of sciences, KoSice Institute of Physics of Materials, Academy of Sciences of the Czech Republic, Bro DFPM 26-29 october 2014 Stara LesnaSoft magnetic composites Composites consisting of soft magnetic powder Soft Ferrites and dielectric bond is applied in DC and AC Inductor cores, transformer cores and other choke cores in switched mode power supplies, applications where electro-magnetic materials noise filters, cross-over filters for loudspeakers, are required to operate at high frequencies inductors and transformers, axial flux machine, these advantages make Soft Ferrites stator in electric motors... paramount over all other magnetic materials. Improvement of PM SMC — innovative 3D design of electric motors Law Rector hort engevinngs ig ator ooing 98Soft magnetic sintered metals - give good performance for DC applications but their use in Moiivvation high-frequency AC applications is limited by high total losses. - high saturation magnetic flux densities - large area indicating a significant losses JA, Bas et al. | Journal of Magnetism and Magnetic Materials 254-255 (2003 } 391-398 1076 45 3a 18 o -15| “3 -45| 1 0 H (Alem) Fe-3w1%Si tested at SOOM, 5 0 H (Alem) Fein teste at 0.01 Soft magnetic composites — the magnetic characteristic remain relative stable over the wider range of frequencies. 107x6, 45 A B (Teslas) 5 10 sts asi 6 45 3 1 5 3 45 6 1 Insulated material tested at 0.01Hz Insulated material tested at SOOHZ Fig. 15, Hysteresis loops for Fe-3%Si and insulated material, tested at 0.01 and 500 Hz.Composition of soft magnetic composites dielectric organic or compaction inorganic coating thermal treatment Metal powder Organic coating (latest research — phenol formaldehyde resins) Advantage * smart preparation * high density of final green compacts * thermally undemanding curing process max. 400 °C Disadvantage thermal treatment temperature for these materials is strictly limited by the thermal resistance of the organic insulating material which is not high enough for removing some plastic deformations created after compaction step in the green compactInorganic coating Soft magnetic sintered metals oxides in spinel structure Advantage - good high frequency characteristic - high initial magnetic permeability - high electric resistivity which results in low eddy current losses over wide frequency ranges - stability over wide temperature ranges. - ability to conduct electron flow through the material Disadvantage - low saturation magnetic flux densities - difficult to sinter (hard material), thus resulting in a problem obtained material with sufficient density - shrinkage of ferrite during sintering The aim of present work was to create soft magnetic composite powder base on FeSi and Permalloy type substrate and nickel ferrite coating.Formation of NiFe,O, ferrite powder - vital ferrite because of the most technologically important applications - spinel ferrite prepared by wet chemical method from alkaline solution NiCl, + 2NaOH — Ni(OH) , + 2NaCl FeCl, +3NaOH — Fe(OH), +3NaCl [Fe"Fe™ (OH),]+[CLnl1,O] -> Fe(OH) ,(aq) > FeO, (OM), 24 9.4/7 FeO(OH) ox Ni(OH), +2FeOOH > NiFe,0, +2H,O z Foo) Ol suetching vib wansmittance sam wt 100% Feo ‘octadie 4900" 3800” 3000” 2600 2000 1600” 1000 100 200” 300” 400” sh)” ot 70” NO 900) ‘wavenumber (em) temperture 10) FTIR analysis of annealed NiFe,O, TG analysis of NiFe,O, amorphous phaseand RTG analysis of NiFe,O, NiFe,0, 100% Intensity a.u. m0 Position (2) TEM image of NiFe,O, powder, 60 nm RTG diffraction pattern of NiFe,O,Formation of core-shell particles Creation of nano-cuboidal spinel NiFe,O, coating by chemical precipitation from an alkaline bath containing Ni?* and Fe** ions. Experimental procedure 1. Oxide-hydroxides intermediate was mixed with particles of FeSi and Permalloy 2. Decantation of coated particles with precipitate for removing of the rest of chlorides 3. Filtration 4. Annealing at 500 °C for 1 hour SEM Original powders FeSi powder (97% Fe) Permalloy type powder 80% NiFeSi/coating Coated powders Permalloy/coating Cross section of coatings FeSi/coating Permalloy/coatingX-ray analysis Intensity au sFesi 59.7% #NiFe,0, 27.9% FeO, 124% Position (23) XRD pattern of the bilayer coating on FeSi particle Intensity a. Nickel Iron 60.5% 14% 8.1% 0 dy se ON 20 Position (20) XRD pattern of the bilayer coating on P72 particleFIB * Electron image otective platinum layer deposition ough milling of trenches, regular cross section, rut |. lator tip Ect Pere Per * Welding and cut off Ee TT * Extraction of lamella Senin acon * Attaching lamella to ce) a CE Perey ao the TEM gird, final thinning PenuassT FeSi/coating TEM image of cross-section of coating on Fe,Si substrate with adequate diffractograms: zoom a) layer a consisted mainly of Fe,O, and minimum NiFe,O,, zoom b) interlayer b consisted of Fe,0,, zoom c) layer ¢ - SiO, and silicides Fe,Si, zoom d) layer d - Fe,Si substrateFe Spectrum a © 36.41 wi% 0 31.77 m% Si 277 wi% Si 1.45 wi% Fe 60.03 wi% Fe 66.24 wt% Ni 0.79 wt% Ni 0.24 wi% © 24.75 wt% Si 5.63 wt% Fe 70.63 wt% EDX analysis of individual layers in the coating on Fe,Si substrate: spectrum a) of the top layer consisted mainly of Fe,O,and minimum NiFe,O,, spectrum b) interlayer consisted mainly of Fe,O, spectrum ¢) thin layer of SiO, and silicides Fe,Si, spectrum d) substrate Fe,SiTEM coating TEM image of cross- section of coating on Permalloy type substrate powder with adequate diffractograms and EDX analysis from zoom a) the top layer a consisted only of NiFe,O,, zoom b) interlayer b consisted of mainly NiFe,O, an minimum of FEO zoom ¢ ) Permalloy type substrate, layer ¢Conclusions NiFe,O, ferrite as a nano-powder — size 60 nm, spinel structure — can be obtained by precipitation from chloride solution containing Ni?* and Fe** ions in the presence of alkaline environment under exactly defined conditions. NiFe,O, can be created by precipitation in the form of coating only on the substrate with the higher content of Ni— Permalloy type powder The higher affinity of the Fe** ion to the iron base substrate — Fe,Si causes a higher amount of Fe,O, ferrite on the surface. In both cases, the multi-layer coating was created on both used substrates . Sample NiFe,O, Fe,Si/coating P72/coating Notation for layer c b b SiO, Fe,0, compound Pure powder copies NiFe,O, face composition / % 100 - 8 crystalline size / nm 60 2 31Thank you for your attention ©