Effect of Heat Treatment Time on Dy–Cu Alloy Diffusion Process in Dy-Containing Commercial Nd–Fe–B Sintered Magnets

In this paper, the grain boundary diffusion process(GBDP) using a Dy_(70)Cu_(30)(at.%) alloy as the diffusion source was performed in a commercial sintered Nd–Fe–B magnet, and the effect of heat treatment time on the microstructure and magnetic properties of the magnet was investigated in detail. For the processed magnets heat-treated at 860℃, as heat treatment time increased, the coercivity and the depth of(Nd,Dy)_2Fe_(14)B core–shell structure increased first and then decreased. However, when the heat treatment time was more than 2 h, the diffusion path of Dy from the Dy-rich shell phase into the Nd_2Fe_(14)B grains was revealed, and a nearly homogeneous(Nd,Dy)_2Fe_(14)B phase was formed, which brought on the decrease in both the depth of visible core–shell structure and the coercivity of Nd–Fe–B magnet.     

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.     

Precipitate Phases in an 11% Cr Ferritic/Martensitic Steel with Tempering and Creep Conditions

Precipitates in an 11% Cr ferritic/martensitic steel containing Nd with tempering and creep conditions were investigated using transmission electron microscope with energy-dispersive X-ray spectroscopy. The precipitates in the steel with a tempering condition were identified to be Cr-rich M23C6 carbide, Nb-rich/V-rich/Ta–Nb-rich MX carbides, Nbrich MX carbonitride, and Fe-rich M5C2 carbide. Nd-rich carbonitride, which is not known to have been reported previously in steels, was also detected in the steel after tempering. Most of the Nb-rich MX precipitates were dissolved, whereas the amount of Ta-rich MX precipitates was increased significantly in the steel after a creep test at 600 °C at an applied stress of180 MPa for 1,100 h. No Fe2 W Laves phase has been detected in the steel after tempering.(Fe, Cr)2W Laves phase with a relatively large size was observed in the steel after the creep test.     

Non-equilibrium Phases Formed in Cu–In–Se–Te System Synthesized by Melt-Quench Method

Non-equilibrium phases formed in melt-quenched Cu In(SexTe1-x)2system, where x = 0.1, 0.2, 0.4, 0.5, 0.6,0.8 and 0.9, have been studied using Rietveld refinement of the crystal structure and Raman spectroscopy. Results of structure refinement have showed that all the samples, except the Cu In(Se0.1Te0.9)2, are heterogeneous. All the observed non-equilibrium phases are quaternary system and are found to have chalcopyrite structure(I"42d), in accordance with the Cu In Te2–Cu In Se2 phase diagram. The lattice constants deduced from the refinement have showed linear variation with Se content. A detailed analysis of the characteristic A1 modes present in the Raman spectrum of individual sample has corroborated the results obtained from the structure analysis. The position of A1 mode of individual phase is found to vary linearly with Se content, which suggests that Cu In(SexTe1-x)2system exhibits single-mode behaviour.     

Phase selection and performance of Mg–Cu–Y amorphous composite with different Mg/Cu ratios

In this article, Mg–Cu–Y alloys with two different Mg/Cu ratios(in at%) were prepared using a watercooled copper mold. Scanning electron microscopy and X-ray diffraction were applied to analyze the microstructure and phase composition. Moreover, corrosion resistance and wear resistance were studied systematically. The results show that both Mg65 Cu25 Y10 and Mg60 Cu30 Y10 alloys could form a composition of crystalline and amorphous phases. Although the microstructure of Mg65 Cu25 Y10 consists of an amorphous phase and a-Mg, Mg2 Cu, and Cu2 Y crystalline phases, the microstructure of Mg60 Cu30 Y10 alloy mainly consists of the amorphous phase and a-Mg, Mg2 Cu. With reducing Mg/Cu ratio, the alloys have better corrosion resistance and wear resistance. The mechanism has also been discussed in detail.     

Effects of milling and crystallization conditions on microstructure of Nd2Fe14B/α-Fe powder

Effects of milling and crystallization conditions on microstructure,such as amorphous phase and nanocrystalline phase, were investigated by X-ray diffractometry(XRD),differential scanning calorimetry(DSC),and transmission electron microscopy (TEM),respectively.The results show that nanocomposite Nd2Fe14B/α-Fe powder can be prepared by mechanical milling in argon atmosphere and a subsequent vacuum annealing treatment.The grain sizes of both Nd2Fe14B andα-Fe phase decrease drastically with increasing milling time.After milling for 5 h,the as-milled material consists ofα-Fe nanocomposite phases with the grain size of 10 nm,and some amorphous phases,which can be turned into Nd2Fe14B/α-Fe nanocomposite phases by the subsequent annealing treatment.Milling energy of mechanical milling after 5 h by theoretical calculation is 6 154.25 kJ/g.     

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.     

Precipitate Behavior in Fe–20Cr–30Ni–2Nb Austenitic Heat-Resistant Steel

In this study,the precipitation behavior of a new austenitic heat-resistant steel(Fe–20Cr–30Ni–2Nb,in at%)was investigated.The effects of alloying addition of boron(B) and lanthanum(La) on the microstructure of the austenitic steel were scrutinized using SEM,EPMA,TEM,and XRD.The results showed that the addition of B enhanced the precipitation of bar-type Laves phase.A small precipitate with high La concentration was observed at the grain boundary in the alloy without aging;similar precipitates without La also presented in region adjacent to the La single phase.This result indicates that La can exist independently and does not contribute to the formation of new compounds.However,in both Band La-modified alloy,B appeared in the precipitate free zone.In the alloy containing both B and La,only Fe2 Nb Lavesphase precipitates,as indicated by the XRD result.     

Microstructure and melting properties of Ag–Cu–In intermediate-temperature brazing alloys

The microstructure and melting properties of ternary Ag–Cu–In intermediate-temperature alloys(400–600 °C) prepared by electric arc melting were investigated in this work. The melting properties, phase compositions, microstructure and hardness were characterized by differential scanning calorimetry(DSC), X-ray diffraction(XRD), scanning electron microscopy(SEM)and micro-hardness tester, respectively. The results show that the melting properties, phase compositions, microstructure and hardness of Ag–Cu–In brazing alloys are substantially different when adding different levels of indium. Indium element could effectively reduce the melting temperatures of(Ag–Cu28)–x In alloys, and the melting temperatures of(Ag–Cu28)–25In alloy are located at 497.86 and 617.48 °C. When the indium content varies from 5 wt% and 10 wt%, the dominant phases in the alloys are Ag-rich and Cu-rich phases, and their granular crystals are smaller than 0.5 lm. When the indium content is higher than 15 wt%, the phase compositions of the alloy are Ag4 In and Cu11In9, and the microstructure exhibits dendritic crystals with a uniform distribution. The hardness of(Ag–Cu28)–x In alloy decreases first and then increases with the content of indium increasing, and the highest hardness of(Ag–Cu28)–25In alloy is HV 266.0.     

Magnetic properties of sputtered anisotropic Pr–Fe–B thin films with different structures and antiferromagnetic materials

Anisotropic Pr–Fe–B films with soft-magnetic layer(Fe) and/or antiferromagnetic layer(Mn, Fe Mn or Mn O) were prepared by direct-current(DC) magnetron sputtering on Si(100) substrates heated at 650 °C. The influence of four types' different structures on the magnetic properties of Pr–Fe–B films was investigated.The phase and magnetic properties were characterized by means of X-ray diffraction(XRD) and superconducting quantum interference device(SQUID). Addition of antiferromagnetic layer enhances both the coercivity and the remanence ratios of Pr–Fe–B films with suitable structures. The interface number increases and the antiferromagnetic–ferromagnetic exchange interaction is likely to become stronger, which affect the improvement of magnetic properties. To further understand the influence of structures with soft-magnetic Fe layer and/or antiferromagnetic Fe Mn layer on the magnetic properties of Pr–Fe–B hard-magnetic films, the thickness of Pr–Fe–B layer was designed to decrease from 600 to 50 nm. The improvement of magnetic properties becomes obvious in Mo(50 nm)/Pr–Fe–B(25 nm)Mo(2 nm)Fe Mn(20 nm)Mo(2 nm)Pr–Fe–B(25 nm)/Mo(50 nm) film.     

Desorption–recombination behavior of as-disproportionated NdFeCoB compacts by reactive deformation

The disproportionated phases of Nd Hx, Fe2B,and a-Fe from Nd2Fe14B were applied to prepare Nd Fe B magnets by two different routes. The results show that the route of annealing in horizontal vacuum sintering furnace cannot reach the purpose of complete recombination after the hot pressing and hot deformation process due to the lack of dehydrogenation channel. The route of applying low pressure of 4–25 MPa on the as-disproportionated green compact during the desorption recombination process in situ hot deformation in a spark plasma sintering(SPS)system can obtain completely recombined Nd Fe B magnet with good anisotropy and magnetic properties. The maximum magnetic properties,(BH)max= 201 kJ m-3,Br= 1.142 T and Hcj= 469 k A m-1, are obtained after being treated for 15 min at 750 °C under low pressure.     

Effect of Solution Treatment on Microstructure and Corrosion Properties of Mg–4Gd–1Y–1Zn–0.5Ca–1Zr Alloy

The as-cast multi-element Mg–4Gd–1Y–1Zn–0.5Ca–1Zr alloy with low rare earth additions was prepared, and the solution treatment was applied at different temperatures. The microstructural evolution of the alloy was characterized by optical microscopy and scanning electron microscopy, and corrosion properties of the alloy in 3.5% NaCl solution were evaluated by immersion and electrochemical tests. The results indicate that the as-cast alloy is composed of the a-Mg matrix,lamellar long-period stacking-ordered(LPSO) structure and eutectic phase. The LPSO structure exists with more volume fraction in the alloy solution-treated at 440 °C, but disappears with the increase in the solution temperature. For all the solution-treated alloys, the precipitated phases are detected. The corrosion rates of the alloys decrease first and then increase slightly with the increase in the solution temperature, and the corrosion resistance of the solution-treated alloys is more than four times as good as that of the as-cast alloy. In addition, the alloy solution-treated at 480 °C for 6 h shows the best corrosion property.     

High-temperature Oxidation Behavior of a High Manganese Austenitic Steel Fe–25Mn–3Cr–3Al–0.3C–0.01N

In this paper, a Fe–Mn–Al–C austenitic steel with certain addition of Cr and N alloy was used as experimental material. By using the SETSYS Evolution synchronous differential thermal analysis apparatus, the scanning electron microscope(SEM), the electron microprobe(EPMA) and the X-ray diffraction(XRD), the high-temperature oxidation behavior microstructure and the phase compositions of this steel in air at 600–1,000 °C for 8 h have been studied. The results show that in the whole oxidation temperature range, there are three distinct stages in the mass gain curves at temperature higher than 800 °C and the oxidation process can be divided into two stages at temperature lower than 800 °C.At the earlier stage the gain rate of the weight oxidized in temperature range of 850 °C to 1,000 °C are extremely lower.The oxidation products having different surface microstructures and phase compositions were produced in oxidation reaction at different temperatures. The phase compositions of oxide scale formed at 1,000 °C are composed of Fe and Mn oxide without Cr. However, protective film of Cr oxide with complicated structure can be formed when the oxidation temperature is lower than 800 °C.     

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.     

Formation of M_(n+1)AX_n phases in Ti–Cr–Al–C systems by self-propagating high-temperature synthesis

In this paper, phase composition of the Mn+1-AXnphases by self-propagating high-temperature synthesis(SHS) was determined using Ti, Cr, Al, and carbon black as raw materials. And, phase composition and microstructures of the Mn+1AXnphases-contained bulk by SHS with the pseudo-hot isostatic pressing(SHS/PHIP) were investigated in Ti–Cr–Al–C systems raw materials. Rietveld XRD refinement was introduced to study the lattice parameters and phase composition of the resultant phases from the SHSed and SHS/PHIPed samples. Ti2 AlCx,Ti3AlC2x, and Cr2 AlCxby SHS were detected in the Ti–Cr–Al–C systems, as well as the binary carbide of TiC and intermetallics. The mechanical properties of the synthesized bulk samples were determined, exhibiting a high strength and toughness compared with the typical monolithic Mn+1AXnphase ceramics. It is indicated that the samples prepared by SHS/PHIP are identified to be a strategy for improving the mechanical properties of monolithic Mn+1AXnphase.     

Atom Probe Tomography Study of Fe Segregation at Phase Interface in Zr–2.5Nb Alloy

β-Nb is a typical second phase in Zr–Nb-based alloys used as fuel claddings in water-cooled nuclear reactors. The segregation of alloying element Fe may affect the corrosion resistance of Zr–Nb-based alloys. In this work, the Fe segregation at the interface between β-Nb phase and α-Zr matrix in Zr–2.5 Nb alloy was studied using atom probe tomography and focused ion beam. The results suggested that the Fe concentration was much lower than Nb concentration in α-Zr matrix, while Fe selectively segregated at the β-Nb/α-Zr phase interface, leading to a Fe concentration peak at some interfaces. The peak Fe concentration varied from 0.4 to 1.2 at.% and appeared at the position where Zr concentration was approximately equal to Nb concentration. The selective segregation of Fe should be affected by the heat treatment and structure defects induced by cold rolling.     

Microstructure Characterization and Fracture Toughness of Laves Phase-Based Cr–Nb–Ti Alloys

Three Laves phase-based alloys with nominal compositions of Cr2Nb–x Ti(x = 20,30,40,in at%) have been prepared through vacuum non-consumable arc melting.The results show that the microstructures of Cr2Nb-(20,30) Ti alloys are composed of the primary Laves phase C15–Cr2(Nb,Ti) and bcc solid solution phase,while the microstructure of Cr2Nb–40Ti alloy is developed with the eutectic phases C15–Cr2(Nb,Ti)/bcc solid solution.The measured fracture toughness of ternary Laves phase C15–Cr2(Nb,Ti) is about 3.0 MPa m1/2,much larger than 1.4 MPa m1/2for binary Laves phase Cr2 Nb.Meanwhile,the fracture toughness of Cr2Nb–x Ti(x = 20,30,40) alloys increases with increasing Ti content and reaches 10.6 MPa m1/2in Cr2Nb–40Ti alloy.The eutectic microstructure and addition of Ti in Cr2 Nb are found to be effective in toughening Laves phase-based alloys.     

Effect of La and Nd on microstructures and mechanical properties of AZ61 wrought magnesium alloy

Effects of La and Nd addition on the microstructure and mechanical properties of the AZ61 alloy have been investigated. The results show that when La and Nd are added into the AZ61 alloy respectively, the β(Mg17-Al12) phase is refined and granulated, and new phases are formed in the form of small rod-like shape, which are verified as La3 Al12 and Nd3Al11 phase by X-ray diffraction and TEM observation. Microstructure observations show that the effective efficiency of La addition is higher than that of Nd addition, thus the sizes of β(Mg17 Al12) and La3Al11 phase are relatively smaller than those of β(Mg17 Al12 ) and Nd3 Al11 phases in both AZ61 alloy and Nd-containing alloy. The increase of the tensile strength and elongation of AZ61 alloy refers to the existence of small rod-like La3Al11 and Nd3Al11 phases, and fine granulated β(Mg17 Al12 ) phase.     

Bainite isothermal transformation of Si–Mn–Mo alloy by phase structure factor calculation under different rare earth contents

The effect of rare earth(RE) on bainite transformation mechanism is not yet unified in the academia.Therefore, further studying the effect of RE on bainite transformation mechanism will have important guiding significance for the development of bainite steels. In this paper, using differential dilatometer(DIL805A/D), heat treatment was performed and C-curve was drawn. The effect of phase structure factor on bainite transformation under two different fractions of RE in Si–Mn–Mo bainite steels was investigated by the empirical electron theory(EET) of solids, molecules, dilatometry, and metallography. Experimental results show that RE makes Fe–CRE segregation structural unit of Si–Mn–Mo bainite steels increase, i.e., the values of phase structure factor(nA, FDC)increase, and delay bainite transformation due to the drag effect resulting from the segregation of RE ferrite island interphase and the retardation of RE to carbon diffusion in Si–Mn–Mo bainite steels. Beside this, C-curve is shifted to right and down, and microstructures of bainite ferrite and substructures are finer.     

The Minor Precipitation at the Final Stage of U720Li Solidification

The minor precipitations caused by B and Zr which are the normal constituents of U720 Li alloy have been studied by analyzing the solidification process and the composition evolution. The present study aims to supply the elementary information about the existing form of B and Zr in the as-cast microstructure, which is helpful for the subsequent processing, such as homogenization treatment. The M_3B_2 and Ni_5Zr phases were observed in the U720 Li alloy in as-cast state, which were usually accompanying with each other together with g-Ni_3 Ti phase at the edge of eutectic(γ+γ'). Combining the DTA analysis and heating and quenching tests, the solidification sequence was determined to be the following: c matrix, eutectic(γ+γ'), g-Ni_3Ti, M_3B_2 and Ni_5Zr. The in situ composition analysis by EDS and EPMA revealed that the precipitation and microstructure were governed by the composition evolution in the liquids. The solidification of c matrix increased the Ti concentration in the residual liquids and resulted in the eutectic(γ+γ') formation; the(γ+γ') formation increased the Ti/Al radio in the liquids and the g-Ni_3Ti was formed in front of the eutectic(γ+γ'); the g-Ni_3Ti precipitation consumed up Al and Ti and increased the concentration of B, Mo and Cr, and M_3B_2 boride is formed;the previous precipitation of the phases consumed up most of the elements other than Ni and Zr, and Ni_5Zr is formed finally. The melting points are in the ranges of 1130–1140 °C for Ni_5Zr phase, 1180–1190 °C for M_3B_2 boride and1190–1200 °C for g-Ni_3Ti phase.