Effect of Post Annealing on the Microstructure and Magnetic Properties of NdFeB/α-Fe/NdFeB Thin Films

A series of nanocomposite thin films, composed of Nd2Fe14B and α-Fe, has been prepared by DC-magnetron sputtering combined ion beam sputtering onto Si (100) substrates. The effects of post annealing on the microstructure and magnetic properties of [NdFeB/α-Fe/NdFeB]-type thin films have been investigated. The X-ray diffraction (XRD) study showed that annealing of the films for 30min at temperatures 550,600,650,700℃ resulted in the appearance of diffraction peaks, characteristic for Nd2Fe14B tetragonal structure, α-Fe and Nd2O3 phases. The investigation using the Vibrating Sample Magnetometer (VSM) with a maximum applied field of 2 T indicated that with the increase of the annealing temperature, the magnetic properties of the multilayer films were improved and reached peak value at 650℃ (Hci=41.72kA·m-1, Mr/Ms=0.4, (BH)max=30.35kJ·m-3), after which the magnetic properties were decreased greatly. Along with the increase of the thickness of α-Fe layer from Tα-Fe16nm, the coercivity Hci, saturation magnetization Ms, and remanence ratio Mr/Ms all declined. As the Atomic Force Microscope (AFM) indicated, after being annealed at 650℃ for 30min, the sample was showed fine surface morphology with grain size 60nm≤dα-Fe≤80nm and 100nm≤dNdFeB≤150nm.     

Influence of Magnetic Annealing on Properties of SmFe Thin Films

SmFe thin films were prepared by DC magietron sputtering at room temperature and 300 %. The influence of magnetic annealing temperature on the phase structure and magnetic properties was investigated. Results showed that thermal sputtering followed by a heat treatment process helped to obtain a structure with a relatively large fraction of SmFe2. Residual phases observed were α-Fe, Sm2O3, and unknown phases. During the annealing treatment, the intrinsic compressive stress in SmFe films was relieved and could become tensile at higher annealing temperatures. The degree of in-plane anisotropy weakened, and furthermore, the anisotropy transformed into out-of-plane anisotropy.     

Effects of magnetic annealing on crystallization and magnetic properties of Nd2Fe14B/α-Fe nanocomposite magnets

Crystallization and magnetic properties of Nd2Fe14B/α-Fe nanocomposite magnets have been investigated by annealing the as-spun ribbons with magnetic field.The crystallization process was accelerated by field annealing.The hysteresis loop became to be fat by magnetic annealing at 645 oC for 4 min,which was 690 oC for ribbons annealing without magnetic field.The relative content of α-Fe phase was increased from the results of XRD.The strength of the magnetic field had no obvious influence on the remanence and coercivity,but modified the squareness of hysteresis loop.     

Effect of titanium addition on the magnetic property of Nd2Fe14B/α-Fe nanocomposite alloys

Rapidly solidified nanocrystalline α-Fe/Nd2Fe14B alloys with enhanced coercivity were obtained by melt spinning.The effects of Ti addition on the microstructore and magnetic properties of the nanocomposite α-Fe/Nd2Fe14B alloys were investigated by X-ray diffraction(XRD)and superconducting quantum interference device(SQUID)magnetometer.The analysis of XRD showed that Vα-Fe estimated to be about 35.3% in the Ti-free α-Fe/Nd2Fe14B nanocomposites decreased down to 26.5% as the addition of was 5 at.% Ti.Accordingly,adding Ti resulted in relevant improvements of magnetic properties,especially of the coercivity Hc from 595 kA/m up to 1006 kA/m.The dependence of Mirrev(H)/2Mr on the reverse field H indicated that nucleation was the dominating mechanism for the magnetization reversal in these nanocomposites.The analysis of the temperature dependence of the demagnetization curve in the α-Fe/Nd2Fe14B nanocomposite magnets indicated that a reduction of αex could play a leading role in an increase in the coercivity of Ti-doped sample.     

Magnetic and magnetostrictive properties of amorphous TbFefFeAl multilayer thin film

Exchange coupling multilayer thin films, which combined giant magnetostriction and soft magnetic properties, were of growing interest for applications. The TbFe/FeAl multilayer thin films were prepared by dc magnetron sputtering onto glass substrates. The microstructure, magnetic, and magnetostrictive properties of TbFe/FeAl multilayer thin film was investigated at different annealing temperatures. The results indicated that the soft magnetic and magnetostrictive properties for TbFe/FeAlmultilayer thin film compared with TbFe single layer film were obviously improved./n comparison with the intrinsic coercivity JHo of 59.2 kA/m for TbFe single layer film, the intrinsic coercivity jHc for TbFe/FeAl multilayer thin films rapidly dropped to 29.6 kA/m. After optimal annealing （350 ℃×60 min）, magnetic properties of Hs=96 kA/m and jHc=16 kA/m were obtained, and magnetostrictive coefficient could reach to 574×10^-6 under an external magnetic field of 400 kA·m^-1 for the TbFe/FeA1 multilayer thin film.     

Differences of element distribution between free and wheel side surface of NdFeB/α-Fe ribbons

The ribbons of NdFeB/α-Fe composite alloy were prepared by melt spinning and post crystallizing technique.The element distri-butions and phase component of both surfaces of as-spun ribbons were measured by energy dispersive spectrometry (EDS) and X-ray diffrac-tion (XRD).Because of the centrifugation,a segregation of B,Fe,and Nd concentrations was observed at the cross section.After crystallizing annealing,the element concentration segregation still existed in the as-crystallized ribbons.Due to the segregation of B,Fe,and Nd,the B-rich phase was observed near the wheel side surface.The B-rich phase may deteriorate the magnetic property of NdFeB/α-Fe composite alloy.     

Hydrogen Embrittlement Processes and AL／AL2O3 Hydrogen Resistance Coatings of NdFeB Magnets

After analyzing the phenomena and processes of hydrogen embrittlement of NdFeB permanent magnets, RF magnetron sputtering was used to fabricate A1 thin films and then oxidized to form the Al/Al2O3 composite films on the magnets as the hydrogen resistance coatings. SEM and EDS were used to examine the morphology and composition respectively. Hy-drogen resistance performance was tested by exposing the magnets in 10 MPa hydrogen gas at room temperature. The results show that the magnets with 8μm Al/Al2O3 coatings can withstand hydrogen of 10 MPa for 65 min without being embrittledinto powd er. The samples with and without hydrogen resistance coatings have almost the same magnetic properties.     

Crystal structure,microstructure and magnetic properties of SmCo-based films treated by different annealing methods

Effect of conventional thermal annealing(CTA) and rapid recurrent thermal annealing(RRTA) processes on crystal structure,mi-crostructure,and magnetic properties of the SmCo-based films were investigated.The results indicated that the CTA-treated films exhibited poor permanent magnetic properties,and a low intrinsic coercivity of 72.8 kA/m was observed.Wide hysteresis loop was obtained for the RRTA-treated films,providing better permanent magnetic properties.The intrinsic coercivity reached 312.0 kA/m.According to the X-ray diffraction(XRD) and atomic force microscopy(AFM) results,the magnetic properties of the CTA-treated films and RRTA-treated films were found to be correlated with the crystal structure and microstructure,which were strongly determined by the annealing treatment.CTA treatment led to poor crystallization effects for the films,and a rough surface(RMS=3.47 nm and P-V=35.42 nm) and large grain size of 92.7 nm were observed correspondingly.However,the RRTA treatment exhibited great contributions on the crystallization of the films,which is accountable for the smooth surface(RMS=2.047 nm and P-V=16.43 nm) and fine grain size of 60.8 nm.     

Magnetic properties of SmCo-based permanent magnetic films during 25 to 300 ℃

Magnetic properties of the SmCo-based permanent magnetic films prepared on hot substrate with Mo and Cr underlayer without subsequent annealing process were investigated by vibrating sample magnetometer （VSM）, X-ray diffraction （XRD）, and en- ergy dispersive X-ray spectroscopy （EDS）. The results showed that the film thickness of the SmCo-based films presented complex effect on the intrinsic coercivity Hci. Optimal Hc~ for the films with Mo underlayer, Cr underlayer, and without underlayer was ob- served with different film thicknesses. Furthermore, the monotonous temperature dependence of Hci was found to be strongly corre- lated with the magnetic parameters for the 3.0 μm thick SmCo7 films with Mo underlayer. From 25 to 300 ℃, the Hci decreased from 281.6 to 211.2 kA/m with a temperature coefficient of-0.091%/℃, exhibiting good temperature stability.     

Effect of film thickness on magnetic properties of Cr/SmCo/Cr films

Cr/SmCo/Cr films with different SmCo thickness were deposited on glass substrates by magnetron sputtering,followed by an annealing process at 550 °C for 20 min.Experimental results showed that the SmCo film of 30 nm exhibited two-phase behavior in the demagnetization process,the obvious kink was observed near zero.For the SmCo film of 50 nm,the kink was invisible,and a single phase like behavior was obtained in the demagnetization process.The reversal behavior became consistent in the thicker films.Moreover,the coercivity reduced and the saturated magnetization increased obviously with the increasing thickness.X-ray diffraction results indicated that the average grain size of SmCo 5 in the thicker films were almost 30 nm,but the quantity of SmCo 5 grains increased with the increasing thickness,which enhanced the intergrain exchange coupling(IEC) of the SmCo 5 hard phases.The increase of IEC improved the magnetic properties of SmCo films with increasing thickness.     

Effect of magnetic layer thickness on magnetic properties of Ce-Fe-B thin films

The Ce_2 Fe_(14)B thin films with a notable out-of-plane c-axis texture were prepared by DC magnetron sputtering on a Ta buffer layer. The morphological and magnetic properties were investigated. The thickness of the magnetic layer had a dramatic effect on the formation of Ce_2 Fe_(14)B phase,and excellent magnetic properties(H_(ci)≈4.25 kOe, M_r/M_s≈0.81) were observed for the Ce-Fe-B film with the thickness d_m = 200 nm. The results of the hysteresis loops for Ce-Fe-B film(d_m = 200 nm) at various measured temperatures show that a decoupling between the hard and the soft phases is observed at low temperatures, which is due to the regions with quite low anisotropy provided by the a-Fe. Moreover. it is clear that significantly various magnetization behaviors between the films with d_m = 200 and 300 nm were observed with a similar trend due to the existence of the a-Fe soft phase.     

Effect of Cobalt on HDDR Anisotropic NdFeB

The effect of cobalt on the magnetic properties and anisotropy of HDDR anisotropic NdFeB was studied.It is found that Co is helpful for preparing anisotropic NdFeB with high coercivity. The research on the initial microstructure for NdFeB alloy indicates that Co tends to enter the crystal lattice of Nd-rich phase and some of Co atoms also enter the crystal lattice of Nd2Fe14B. The dissolution of Co changes the stability of Nd-rich phase and Nd2Fe14 B in H2 atmosphere and affects the kinetics of HDDR phase transformation. As a result, the NdFeB powder exhibits a high coercive force and a strong anisotropy.     

Dependence of Magnetic Properties of Rapidly Quenching （Nd, Pr）x（FeCoZr）94-xB6 Bonded Magnets on Rare Earths Content

By using sub-everquenching and annealing method which has a wide processing window, (Nd, Pr)x(Fe-CoZr)94-xB6(x=12, 10.5, 10, 9) bonded magnets were prepared and the effect of rare earths content on magnetic properties was investigated. Being spun at sub-ove, quenching speed the as-spun ribbons consist of amorphous phases mixed with fine crystallites. After crystallization under optimum annealing conditions and bonded with 3.25%(mass fraction) epoxy, the magnets obtained the optimum magnetic properties. The rare earths content directly determines the magnetic properties. With the reduction of rare earths content, Br increases but Hci and (BH)max decrease, x=10 is the critical value for the magnetic properties change. Below this value, Br increases slowly meanwhile Hci and (BH)max decrease strongly because alloy contains extra fractions of soft magnetic phase which are not coupled with the hard magnetic phase. This experimental result is consistont with the calculated results using the model of volume fraction of soft magnetic phase coupled completely suggested.     

Differences in the structure and magnetic properties of(Nd_(0.75)Pr_(0.25))_(9.5)Fe_(76)X_4B_(10.5)(X=Nb,Zr) ribbons by conventional and microwave-assisted annealing treatment

Amorphous ribbons with(Nd_(0.75)Pr_(0.25))_(9.5)Fe_(76)X_4B_(10.5)(X=Nb, Zr) nominal composition were annealed by conventional and microwave-assisted annealing furnaces, respectively. The thermal decomposition process, structure and magnetic properties of products were characterized by a thermal differential scanning calorimeter(DSC), X-ray diffraction(XRD) and a vibrating sample magnetometer(VSM). The addition of Nb and Zr increased the glass-forming ability(GFA) of as-spun ribbons. The proportion of Nd_2Fe_(14)B and α-Fe could be adjusted with power from 800 to 2000 W in microwave annealing process, during which the well-coupling between the soft and hard magnetic phase and higher coercivity reached up to 780.2 and 815.4 kA/m for(Nb,Zr)-doped alloys. The best magnetic properties of ribbons could be obtained by annealing at 650 oC for 10 min under the microwave power of 2000 W.     

Effect of Gallium Addition on Magnetic Properties of Nd2Fe14B-Based/ α-Fe Nanocomposite Magnets

The influence of Ga addition on the crystallization behavior and the magnetic properties of nanocomposite Nd2Fe14B-based/α-Fe magnets was investigated. It was found that the addition of 0.2% did not change the crystallization temperature of amorphous alloy, but the magnetic properties were improved significantly because of the strong exchange coupling interaction between the hard and soft magnetic phases. The optimum magnetic properties with iHc = 600. 3 kA· m^-1, B r = 0.75 T, and （BH）max = 88.03 kJ· m^-3 were obtained in bonded Nd9.5（FeCoZr）83.8 Ga0.3 B6.5 magnet with 15 m·s^- 1 wheel speed and 670 ℃ annealing treatment. The apparent improvement of magnetic properties originates from the grain refinement calculated using the Scherrer formula from corresponding XRD patterns and the excellent rectangularity of the demagnetization curve.     

Coercivity enhancement of Nd2Fe14B/α-Fe nanocomposite magnets through neodymium diffusion under annealing

The coercivity enhancement of ball-milled Nd2Fe14B/α-Fe nanocomposite magnets was investigated. It was found that the coercivity could be enhanced through mixing a small amount of Nd powder with as-milled Fe-rich Nd-Fe-B powders. The annealed samples were investigated by means of X-ray diffraction, scanning electron microscopy and magnetic measurement systems. Under annealing, some of Nd powders promoted the formation of hard magnetic phase Nd2Fe14B. On the other hand, a few of Nd would diffuse into the interface of Nd2Fe14B/α-Fe nanocomposite to compensate for the loss of the interfacial magnetic anisotropy. These two features are all beneficial to the coercivity.     

Effects of Nd Doping on Magnetic-Optical Properties of GdFeCo Thin Films

The GdFeCo and NdGdFeCo thin films were prepared by sputtering, and their hysteresis loops, the temperature dependence of the saturation magnetization Ms and the magneto-optical Kerr spectrum in the visible light range were measured. By studying the effects of light rare earth element Nd doping on the magneto-optical Kerr rotation angle of GdFeCo thin films, it is found that proper Nd additives in GdFeCo films could enhance Kerr rotation at short wavelengths. So it could be better medium used as the readout layer of center aperture detection magnetically induced super resolution （CAD-MSR）.     

Structure and hard magnetic properties of TbCu7-type SmFe8.95−xGa0.26Nbx nitrides

Nanocrystalline SmFe_(8.95-x)Ga_(0.26)Nb_xN_δ(x=0, 0.1, 0.2, 0.3) were prepared using rapid-quenching,annealing and nitriding. The magnetic properties and crystal structures were systematically studied under various wheel velocities to investigate the influence of Nb doping for the compounds. It is found that TbCu7-type structure is able to be obtained even though the wheel velocity is reduced to 20 m/s(x = 0.3). An significant increase(△T_c=70 ℃) of the Curie temperature is obtained with Nb doping at x = 0.1 due to the lattice expansion revealed by Rietveld analysis. The optimum coercivity with the value H_(cj) of 810 kA/m is achieved at x = 0.2 in the nitrides, in which a reasonable distribution of grain sizes of both TbCu_7-type SmFe_9 N_δ and α-Fe can be found. However, an excess of Nb doping may lead to the increase of the weight fraction of α-Fe, which in turn deteriorates the magnetic properties.     

Preparation and Magnetic Properties of Melt-Spinning Nd2Fe14B/α-Fe Nanocomposite Magnets

Nd11Fe71Co8V1.5Cr1B7.5 magnet was prepared by melt-spinning and subsequently annealed. The effects of the wheel speed on the magnetic properties and microstructure were studied. The results reveal that fine nanocomposite microstructure consisting of Nd2Fe14B and α-Fe phases can be developed at an optimum wheel speed of about 21 m·s-1. After optimal annealing (640 ℃×4 min), magnetic properties of Br=0.64 T, jHc=903.5 kA·m-1 and (BH)max=71 kJ·m-3 were obtained for the bonded magnets. The addition of Cr element significantly reduces grain size, increasing the intrinsic coercivity and maximum magnetic energy product.     

Effect of Ti cap layer thickness on microstructures and magnetic properties of Ti/Ni/Ti films

Nanogranular Ti(3 nm)/Ni(30 nm)/Ti(t nm )(t=1,3,5,7,10) films were prepared by facing magnetron sputtering from Ti and Ni onto glass substrates at room temperature.The structural and magnetic properties of films strongly depended on the Ti layer thickness.X-ray diffraction(XRD) patterns of all as-deposited films showed strong FCC Ni(111) peak.Vibrating sample magnetometer(VSM) measurements indicated that the perpendicular coercivity of the Ti(3 nm)/Ni(30 nm)/Ti(3 nm) film reached about 36 kA/m.With the increase of Co layer thickness,coercivity(Hc) first increased and then decreased.The grain size and magnetic clusters slightly increased and the value of roughness(Ra) was smallest at t=3 nm.