Effects of Zr on crystallization kinetics of Pr—Fe—B amorphous alloys

The effects of Zr on crystallization kinetics of Pr-Fe-B amorphous alloys have been investigated by DTA and XRD methods.It was found that for Pr8Fe86-xZrxB6(x=0,1,2)amorphous alloys,the final crystallized mixture is α-Fe and Pr2Fe14B,and the metastable Pr2Fe23B3 phase occurs during crystallization of Pr8Fe86B6 amorphous alloy,not during crystallization of Pr8Fe86-xZrxB6(x=1,2)amorphous alloys,By analyzing the activation energy of crystallization,the formation of an α-Fe/Pr2Fe14B composite microstructure with a coarse grain size in annealed Pr8Fe86B6 alloy,is attributed to a difficult nucleation and an easy growth for both the α-Fe and Pr2Fe14B in the alloy.The addition of Zr can be used to change the crystallization behavior of the α-Fe phase in Pr-Fe-B amorphous alloy,which is helpful to reduce the grain size for the α-Fe phase.     

Structure and magnetostriction of Tb0.4Nd0.6(Fe0.8Co0.2)1.90 alloy prepared by solid-state synthesis

Mechanical alloying (MA) and subsequent solid sintering process was used to prepare the Nd-containing magnetostrictive Tb0.4Nd0.6(Fe0.8Co0.2)1.90 alloy. The structure, thermal stability and phase transformation were investigated as functions of composition, milling process and annealing temperature. An amorphous phase was formed by high-energy ball milling for 5 h with the ball-to-powder weight ratio of 20:1, which crystallized into MgCu2-type and PuNi3-type crystalline structure with different annealing temperatures. The magnetoelastic properties were investigated by means of a standard strain technique. The high Nd-content (Tb,Nd)(Fe,Co)2 Laves phase for the composition Tb0.4Nd0.6(Fe0.8Co0.2)1.90 was synthesized by MA process plus annealing at 500 ℃ for 30 min.     

Microstructure of explosively compacted Nd-Fe-B magnet by TEM

The microstructure of an explosively compacted Nd-Fe-B permanent magnet(Nd-Fe-B) was investigated by means of TEM and XRD. It is shown that there are three kinds of phases: Nd2 Fe14 B matrix phase, O-rich phases and Nd-rich phase with different structures and compositions in the magnet. The hard magnetic phase Nd2Fe14 B is tetragonal, which lattice parameters are determined to be a=0.88 nm and c=1.22 nm. The O-rich phase locates at the grain boundaries and the triple junctions has fcc structure whose lattice parameter is a=0. 559 nm. A dislocation is observed in this phase. It is also found that a large number of the block-shaped Nd-rich phases with hcp structure are embedded in the Nd2 Fe14 B matrix or at grain boundary. Their lattice parameters are determined to be a= 0. 395 nm and c=0. 628 nm.     

Magnetic properties of Nd_2Fe_(14)B/α-Fe nanocomposite magnets with yttrium addition

The phase evolution and magnetic properties of Nd9?xYxFe72Ti2Zr2B15 (x = 0,0.5,1,and 2) melt-spun nanocomposite ribbons were studied.It is found that Y addition not only enhances the formability of amorphous phase in the alloy,but also stabilizes the amorphous phase during the annealing treatment.The appropriate content of Y addition effectively enhances the remanence (Jr) of the annealed sample.The residual amorphous intergranular phase in the annealed sample optimizes the squareness of the loop,resulting in an larger maximum energy product (BH)max.The best magnetic properties,Jr = 0.78 T,Hci (coercivity) = 923.4 kA/m,and (BH)max = 98.5 kJ/m3,were obtained from the Nd8YFe72Ti2Zr2B15 ribbon spun at Vs = 4 m/s and annealed at 700°C for 10 min,which is composed of Nd2Fe14B,α-Fe,and amorphous phase.     

Effect of Annealing on the Magnetism of the Sintered NdFeB Magnet

This paper deals with the effect of annealing on the magnetism of the sintered NdFeB magnet with a composition of Nd30B5.1Dy1.2Al0.6Nb0.7Fe62.4. Microstructural investigations of the grain size and grain boundaries with SEM were carried out. Microstructural investigations showed the presence of some Nd-rich phase in grain boundaries and main phase.The results of magnetic properties analysis shows that this non-magnetic Nd-rich phase, produced in annealing process,can increase or decrease the magnetism of the sintered NdFeB-type permanent magnet. Appropriate amount of Nd-rich phase will strengthen the pinning field and elevated the coercive force of magnet, but too many these non-magnetism phases in Nd2Fe14B main phase will decrease it. When the sintered NdFeB magnet was annealed at 3Pa and 492℃ for an hour the coercive force would raise from 915.6kA/m to l164.SkA/m, and the (BH)max from 277.7kJ/m to 349.5kJ/m. However, annealing at a non-optimized temperature at 542℃, microstructure changes in some main phase will leading the decrease of properties.     

Influence of zirconium addition on the microstructure and magnetic properties of nanocomposite Nd10.1Fe78.2-xCo5ZrxB6.7 permanent magnets

Nanocomposite Nd10.1Fe78.2-xCo5ZrxB6.7 （x= 0, 1.5, 2.5, 2.7, 3, 4） permanent magnets were prepared by melt-spun and annealing. The microstructure and magnetic properties of the permanent magnets were investigated. The resuits reveal that the addition of Zr element significantly reduces the grain size and improves the thermal stability of the amorphous phase. A fme nanocomposite microstructure with an average grain size of about 35 nm can be developed at a wheel speed of 16 m·s^-1 with the content of Zr up to 2.7 at.%. After optimal annealing （710℃ x 4 min）, the magnetic properties of the Ndl0.1Fe75.5Co5Zr2.TB6.7 bonded magnets were achieved as follows： Br= 0.72 T, jHc = 769 kA·m^-1, and （BH）max = 85.0 kJ·m^-3.     

Synthesis of TiAl-Ti2AlN composites by in-situ crystallization

The amorphization process during mechanical alloying （MA） was investigated for the Ti-50%/Al （mole fraction） powder mixtures with no special protection conditions. During the milling process, with the milling time prolonging, the metallic powder Ti and Al were finely mixed, gradually, aluminum completely dissolved into titanium to form an Ti（Al） hcp supersaturated solid solution, and finally, transformed to the amorphous phase after milled for about 39 h. As a result of heat treatment in hot press sintering processing for the mechanically alloyed amorphous powders in vacuum, a submicrostructure intermetallics of TiAl/TizAIN composite can be produced by in-situ crystallization. Furthermore, the structure evolution, phase formation and transformation during the heat treatment were also investigated by X-ray diffractometry and differential thermal analysis. The results show that the reaction involves many transitional stages, including formation of TiAl3 and transformation into TiAl and Ti3Al. The examination show that the composite materials fabricated by this in-situ crystallization from amorphization have good mechanical properties due to fine grain size and uniform microstructure.     

Succession law of Nd–Fe–B alloys with different coercivities

In order to establish a succession law of every phase in sintered Nd–Fe–B magnets marked as 38/38H/38SH/38 UH, four alloys of Nd33-xDyxAl0.7Nb0.6Cu0.1B1.05 Fe bal.(at%) were investigated after smelting processing, sintering processing, high-temperature tempering processing, and highand low-temperature tempering processing. It is found that the four phases: the Nd2Fe14B matrix phase, Nd-rich phase,B-rich phase, and defect phase can be inherited by means of the subsequent processing. These phases might have the special constitution and appearance in the different states.Magnetic properties also have succession law. In every processing except smelting one, the values of remanence and maximum energy product hardly alter, but the value of coercive force increases gradually.     

Effect of preannealing on crystallization process of amorphous Sm5Fe80Cu1Si5B3C2.5Zr3.5 alloy

In the view of crystallization activation energy of amorphous alloy,the mechanism of coarse grain in annealed Sm5Fe80Cu1Si5B3C2.5ZR3.5 amorphous alloy was analyzed.It reveals the e4ffect of preannealing on the process crystallization.The results show that preannealing can be used to change the crystallization behavior of the α-Fe phase in the Sm5Fe80Cu1Si5B3C2.5Zr3.5 amorphous alloy,whick is helpful for forming α-Fe phase grains;and it is not large for Sm2Fe17Cx phase.     

Effect of ball milling process on the microstructure of titanium-nanohydroxyapatite composite powder

Titaninm-nanohydroxyapatite （Ti-nHA） composite powders, composed of titanium with 10 vol.% and 20 vol.% of nano-hydroxyapatite, were milled in a planetary ball mill using alcohol media to avoid excessive heat. XRD and SEM were performed for characterization of the microstructure, and the homogeneity of Ti/HA nanocomposite powder was evaluated by EPMA with prolonged ball milling time. The results show that under the condition of wet milling, the grain size of Ti-nHA composite powders is decreased with the increase in ball milling time and the amount of the addition of nHA. While for milling of 30 h, the nanocomposite powder with free structure, which consists of the nano-hydroxyapatite （nHA） particles and titanium （Ti） phase, is obtained. Three stages of milling can be observed from the dement mapping of Ti, Ca, and P by EPMA; meanwhile, it is found that the nHA would be more homogenously distributed after milling for 30 h.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites （ Ⅱ ）： Structural evolution and grain growth kinetics of mechanically alloyed Fe-Al-Ti-B composite powder during heat treatment

Morphological changes, structural evolutions and grain growth kinetics of mechanically alloyed（MAed） Fe50Al50, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 （mole fraction, %） powders were investigated by XRD and SEM, when being isothermally annealed at 1 073-1 373 K. The effect of different Ti and B addition on the grain growth of FeAI phase was also discussed. The results show that the nanocrystalline FeAI and in-situ TiB2/FeAl nanocomposite powders can be synthesized by subsequent heat treatment. Besides the relaxation of crystal defects and lattice stress, the transformation from Fe-based solid solution into B2-FeAl and TiB2 occurs upon heating of the MA-processed alloys. Although the grain growth takes place, the grain sizes of both FeAl and TiB2 are still in nanometer scale. The activation energies for the nanocrystalline FeAl growth in the three alloys are calculated to be 534.9, 525.6 and 1 069.6 kJ/mol respectively, according to kinetics theory of nanocrystalline growth. Alloys with different TiB2 contents exhibit unequal thermal stability. The presence of higher content TiB2 plays significant role in the impediment of grain growth.     

Magnetic properties optimization of nanocomposite Nd9Fe85B6 magnets by controlling microstructure of as-quenched ribbons

To optimize the magnetic properties of nanocomposite Nd9Fe85B6 magnets, the as-quenched ribbons with different microstructures were prepared at six wheel velocities from 10 to 30 m s-1through rapid quenching,followed by a series of annealing treatments at 550–800 °C for 5–10 min. It is found that both the large initial grains at low cooling rate and high content of amorphous phase at high cooling rate cause a-Fe grains coarsening, which leads to a decline in the strength of exchange coupling interaction and the deterioration of magnetic properties. In order to optimize the magnetic properties, the as-quenched ribbons should be chosen with relatively small initial grains as well as a small amount of amorphous phase. For nanocomposite Nd9Fe85B6 materials, the optimized magnetic properties of Hcj= 446 kA m-1, Br= 0.86 T,(BH)max=80 kJ m-3are obtained for ribbons prepared at 18 m s-1after annealing at 620 °C for 5 min.     

Interfacial defects of hard magnetic Pr2Fe14B phase from amorphous to nanostructures

The interfacial defects of hard magnetic Pr2Fe14B phase from amorphous to nanostructures have been investigated by positron lifetime spectroscopy. The nanostructure was produced by melt-spinning and nanocrystallization route. The two main components can be ascribed to vacancy-like defects in the intergranular layers or the interfaces, and microvoids or large free volumes with size compared to several missing atoms at the interactions of the atomic aggregates or the crystallites. The remarkable changes in the positron lifetimes from the amorphous structure to the nanocrystructure with varied sizes can be interpreted, indicating that the structural transformation and the grain growth induce the defect changes occurring at the interfaces with different shapes and sizes.     

Effect of post annealing on phase transformation of Ni-Mn-Ga ferromagnetic shape memory alloy particles prepared by ball milling

The effect of post annealing on the phase transformation of Ni52Mn24Ga24 ferromagnetic shape memory alloy particles prepared by ball milling was studied. Ni52Mn24Ga24 alloy particles at micron scale were prepared successfully by ball milling the crushed bulk alloy. SEM observation reveals that the shape of the as-milled particle is regular polygon and a lot of cracks can be seen at the surface of the particles. For as-milled particles, the widening of characteristic peak can be found in the XRD pattern, and no transformation characterization can be detected by DSC. Post annealing at the elevated temperature will recover the transformation behavior of milled particles to the same level as that of bulk sample. It is shown that with increasing annealing temperature above 400 ℃, Ms decreases and As increases, while the magnetic transition temperature keeps constant. XRD results indicate that the change of grain size of the particles results in such an effect of post annealing.     

Mcrostructure of TiAl alloy prepared by intense plastic deformation and subsequent reaction singering

TiAl alloy was prepared by intense plastic deformation and subsequent reaction sintering.The effect of plasetic deformation on the microstructure of sintered TiAl alloy was investigated using energy dispersive X-ray spectroscopy(EDS),optical microscopy and transmission electron microscopy(TEM).The results show that the intense plastic deformation of reacting Ti and Al phases caued by high energy ball milling refines the as-sintered microstructure.The longer the milling time,the finer the grain size of γ and lamellar(α2 γ）phases.The finer grain size improves the properties of the TiAl alloy.It is also found that th volume fraction of lamellar(α2 γ)phases increases first,then decreases with increasing milling time.Based on the experimental results theoretical discussion was presented.     

Preparation technology and magnetic properties of Nd9.5Fe77B6Co5Zr2.5 nanocomposite magnets

The preparation technology and magnetic properties of Nd9.5Fe77B6Co5Zr2.5 nanocomposite magnets were investigated by melt spinning and crystallization process. The nonuniform composition and grain size can be induced by nanocomposite magnet prepared by arc-melt-spinning process, which will decrease the magnetic properties. These can be avoided by modification of preparing process. Induction-melt-spinning furnace was designed successfully and applied to prepare nanocomposite magnets. The bonded magnet with Br=0.736, Hcb=418 kA/m, Hcj=630 kA/m, Mr/Ms=0.7 and （BH）max=82.4 kJ/m^3 was prepared by this technology.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites（ Ⅰ ）： Mechanical alloying of Fe-A1-Ti-B composite powder

Three nanocrystalline alloys, FesoAlso, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 （molar fraction, %）, were synthesized from elemental powders by high-energy ball milling. The structural evolutions and morphological changes of the milled powders were characterized by X-ray diffractometry（XRD）, transmission electron microscopy（TEM） and scanning electron microscopy（SEM）. The effects of different Ti, B additions on the structure and phase transformation in these alloys were also discussed. It is observed that the diffusion of AI, Ti, B atoms into Fe lattice occurs during milling, leading to the formation of a BCC phase identified as Fe（Al） or Fe（Al, Ti, B） supersaturated solid solution. Fe-based solid solution with nanocrystalline structure is observed to be present as the only phase in all the alloy compositions after milling. Furthermore, the contents of Ti, B affect the formation of mechanical alloying products, changes in the lattice parameter as well as the grain size.     

Synthesis of TiAl-Al2O3 composites by high energy milling and hot-press sintering

A sub-microstructure titanium aluminide alloy/Al2O3 （3A） composite was obtained by crystallization of the amorphous powders, which were prepared by mechanical alloying （MA） in a planetary ball milling system using Ti-AI-TiO2 as raw materials. The experimental results show that, when the milling time increases up to 30 h, the hep Ti（Al） supersaturated solid solution disappears, only amorphous phase is left. The compact samples were synthesized by hot-press to 1 200 ℃ with the amorphous as a precursor; the final phases of the matrix and strengthened phase are y-TiAl and Al2O3. The phases come from in situ crystallization and transformation. The samples, fabricated from the amorphous phase by hot press sintering, have high bending strength and fracture toughness.     

Magnetic properties and microstructure of nanocomposite(Nd,Pr)–Fe–B ribbons by doping Nb element

Effects of Nb addition and annealing treatmen on magnetic properties and microstructure of(Nd0.4Pr0.6)9Fe76–xNbxB15(x = 0–4) ribbons were systematically investigated by means of vibrating sample magnetometer(VSM) and X-ray diffraction(XRD). The extra phases with nonmagnetic(Nd,Pr)1.1Fe4B4phase and metastable compound(Nd,Pr)2Fe23B3 crystallized during quenching the Nb-free alloy. Moreover, the nonmagnetic(Nd,Pr)1.1Fe4B4phase does not diminish during the following annealing treatment. The addition of Nb to(Nd,Pr)–Fe–B alloy suppresses metastable(Nd,Pr)2Fe23B3 and nonmagnetic(Nd,Pr)1.1Fe4B4phases. The intrinsic coercivity increases from 397 kA m-1for the Nb-free sample to1,091 kA m-1for the 4 at% Nb-doped sample optimally annealed. The Nb-free sample has the magnetic properties with Js= 1.04 T, Jr= 0.66 T, and(BH)max= 43.5 kJ m-3By comparison, the magnetic properties of the 4 at% Nbdoped sample were 0.97 T, 0.68 T, and 65.7 kJ m-3respectively. The significant improvement of magnetic properties mainly originates from the finer grains of the ribbons by introducing Nb.     

Effect of high magnetic field on the crystallization of Nd2Fe14B/α-Fe nanocomposite magnets

Nd8.1Dy0.9Fe76.95Co8.55B5.5 nanocomposite magnets annealed with and without a 10 T magnetic field were investigated in this article. The ribbons with coexisting amorphous and crystalline phases were selected to do this study. The resuits of Moessbauer spectroscopy revealed that the content of α--Fe increased when annealed in high strength magnetic field. The size of the grains also increased considerably after the application of magnetic annealing. All these led to the decrease of the magnetic properties, especially the coercivity of the ribbons.