Texture development and grain boundary phase formation in Ce-and Ce-La-substituted Nd-Fe-B magnets during hot-deformation process

In this study,the influence of Ce-and Ce-La-substitution for Nd in Nd-Fe-B magnets on their magnetic and microstructural changes in the course of the hot-deformation process was investigated to gain insight into further reducing the Nd content in fine-grained Nd-Fe-B hot-deformed magnets.We found that the[001]texture and microstructure of the RE-rich grain boundary phases,which are the factors that de-termine the remanence and coercivity of hot-deformed magnets,were deteriorated by the Ce-and Ce-La-substitution.This is because the volume fraction of the RE-rich liquid formed in the grain boundaries during the hot-press and hot-deformation decreased due to the Ce-and Ce-La-substitution,thereby in-creasing the friction between the 2:14:1 grains while the c-axes of grains were aligned by grain rotation and decreasing the RE concentration of grain boundary phases.In particular,the Ce-La-co-substitution further prevented the liquid formation within the grain boundaries of the magnets during hot-press and hot-deformation because the wettability of the RE-rich liquid on the 2:14:1 grains became poor when La was substituted for Nd in the 2:14:1 grains.These results indicate that there is room for further im-provement in both the remanence and coercivity of the Ce-and Ce-La-substituted magnets by intro-ducing additional liquid into the grain boundaries prior to hot-press and hot-deformation.By applying the Nd-Cu infiltration process to the melt-spun ribbons(intermediate infiltration,I-infiltration),both the remanence and coercivity of the Nd-saving(Nd 0.7 Ce 0.3)-Fe-B and(Nd 0.7 Ce 0.225 La 0.075)-Fe-B hot-deformed magnets were successfully improved.

Spheroidization and Ostwald Growth of Carbide in Isothermal Process of Hot-Deformed High Carbon Chromium Cast Steel

In isothermal spheroidizing process,the spheroidization and growth of the carbide formed in hot-deformed high-carbon chromium cast steel at high temperature were investigated.The results showed that the spheroidizing growth of carbide proceeds in such a way that the bigger carbide particles swallow the smaller ones,and the short rhabdoid carbides dissolve and are spheroidized by itself.When the samples were held at 720℃ for more than 3 h,the spheroidization is not obvious.The feature of the process is the size increment and the amount decrement of carbide particles.The empirical equation for growth rate of carbides was obtained.The volume fraction of carbides keeps constant.The growth process agrees well with Ostwald Ripening Law.

MODELLING FOR PREDICTION OF CONTINUOUS COOLING TRANSFORMATION KINETICS OF HOT-DEFORMED AUSTENITE STEEL

On the thermodynamics basis of regular solution sub-lattice model and soperelement model, kinetics basis of Cahn's transformation kinetics theory, and according to Scheil's additivity rule and eoperimental results obtained by thermal dilation method,a prediction model of transformations from hot-deformed austenite to ferrite, pearlite and bainite in low alloy steels, which could be applied to continuoas cooling process, is developed. The calculated transformed junctions of each phase based on laboratory controlled rolling and controlled cooling conditions in a low alloy steel are in reasonable agreement with the measured ones.

MATHEMATICAL MODELLING OF PHASE TRANSFORMATION FROM HOT-DEFORMED AUSTENITE IN LOW CARBON STEELS

On the basis of superelement model, Cahn’s transformation kinetics theory and Scheil’s additivity rule, the CCT diagrams and transformation kinetics in low carbon steel were predicted considering both undeformed and deformed conditions. The influence of deformation on phase equilibria and transformation incubation period was evaluated quantitatively. The recrystallization kinetics and the evolution of dislocation density were calculated during continuous cooling. The results show deformation considerably shortens transformation incubation period, accelerates transformation kinetics and makes CCT curve shift leftwards. The calculated CCT diagrams and the volume fraction of each phase are in good agreement with measurements.

Deformation-induced α_2/γ Interfaces in a Hot-deformed Ti-45Al-10Nb Alloy

The structure change of α2/γ interface in a Ti-45Al-10Nb alloy induced by hot deformation was investigated by conventional and high-resolution transmission eIectron microscopy. Two types of hot deformation induced special α2/γ intedeces, coherent intedeces with high density of ledges and semi-coherent α2/γ intedeces were found to be due to the absorption of mobile dislocations into the α2/γ inteface. For the misoriented semi-coherent α2/γ interfaces, the densities of dislocation ledges increase with the misoriented angle between (111)γ and (0001)α2 planes, and 1/3[111] Frank partial dislocations were involved in the dislocation ledges. Formation mechanism of these deformation-induced α2/γ interfaces was discussed to be related to the role of α2/γ interface5 adjusting the deformation as a dislocation sink absorbing the slipping dislocations in the γ phase

FLOW STRESS OF STEEL 55SiMnVB AT HIGH TEMPERATURES AND HIGH STRAIN RATES

Based on the analyses of hot-deformation mechanism of the steel,a new constitutive equation describing the flow stress of steels was derived.The flow stress data of steel 55SiMnVB have been determined at 900—1200℃,strain rates of 1—100s^(-1)and true-strain of 0.08—0.8.An available evaluated formula on the flows tress has been obtained by means of non-linear regression.It can express clearly the physical process of hot-deformation.

IMPROVED PROCESSING FOR MICROSTRUCTURES AND MECHANICAL PROPERTIES OF A COMMERCIAL PIPELINE STEEL

The transformation productions of hot-deformation simulation experiments were investigated using a Gleeble-1500 hot simulator for a commercial pipeline steel. Based on the investigation results, the improved thermo-mechanical control processing (TMCP) schedules containing a two stage multi-pass controlled rolling coupled with moderate cooling rates were applied to hot rolling experiments and acicular ferrite dominated microstructure was obtained. Microstructures and mechanical properties of hot rolled plates were related to TMCP processing, and regression equations describing the relation between processing parameters and mechanical properties in the current TMCP were developed, which could be used to predict mechanical properties of the experimental steel during commercially processing. It was found that with an increase in cooling rate after hot rolling, grain size in the microstructure became smaller, the amount of polygonal ferrite decreased and acicular ferrite increased, and accordingly mechanical properties increased.

Coercivity enhancement of hot-deformed Nd-Fe-B magnets with Pr-Cu alloy addition

Effects of low-melting Pr-Cu alloy addition on the microstructure and magnetic properties of the hot-deformation Nd-Fe-B magnets were investigated.A small amount of Pr-Cu addition enhances the coercivity of the hot-deformation Nd-Fe-B magnets obviously.The coercivity of the hotdeformation Nd-Fe-B magnets with 4.0 wt%Pr_(85)Cu_(15)addition increases to 1271 kA·m^(-1),75.69%higher than that of Pr-Cu-free magnet(723 kA·m^(-1)),and then decreases with5 wt%Pr_(85)Cu_(15)addition.It is observed that there a uniform RE-rich phase is formed wrapping the Nd2Fe14B main phase in the sample with 4.0%Pr_(85)Cu_(15)addition by scanning electron microscopy(SEM),which promotes the coercivity.The angular dependence of coercivity for the hot-deformation Nd-Fe-B magnets indicates that the coercivity mechanism is nucleation combined with domain wall pinning.The domain wall pinning is weakened,while the nucleation is enhanced after Pr-Cu addition.Theremanence,intrinsic coercivity,and maximum magnetic energy product of the original Nd-Fe-B magnet are 1.45 T,723 kA·m^(-1),and 419.8 kJ·m^(-3),respectively,and those of the sample with 4.0%Pr_(85)Cu_(15)alloy addition are 1.30 T,1271 kA·m^(-1),and 330.0 kJ·m^(-3),respectively.

Recent progress of grain boundary diffusion process for hot-deformed Nd-Fe-B magnets

Grain boundary diffusion process(GBDP)was first proposed for sintered Nd-Fe-B magnets to achieve the high utilization efficiency of heavy rare earth elements.Recent success of fabricating high performance nanocomposite magnets by GBDP indicates that this method also exerts huge applicable potential on hot-deformed Nd-Fe-B magnets.In this review,the development and magnetic property enhancement mechanisms of different diffusion methods proposed on hot-deformed magnets were thoroughly elucidated.Moreover,the improve room for further property enhancement and the accompanying problems of GBDP on hot-deformed magnets are also discussed in this article.

Development of Microalloyed Medium-Carbon Steel with Improved Toughness

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Microstructure and magnetic properties of anisotropic hot-deformed magnet of different magnetic particle sizes

In this paper, the magnetic Nd-Fe-B particles of different sizes were conducted under vacuum by the hot pressing, then cooled quickly to room temperature. Finally hot deformation was performed to get the anisotropy Nd-Fe- B magnet at a deformation rate of 70 % in the protection of argon atmosphere. NIM-2000 was used for the measurement of hysteresis loop of the samples. Meanwhile, scanning electron microscopy （SEM） was used to observe the surface morphology of the magnetic particles with different sizes and hot-deformed magnets, energy spectrum analyzer to analyze the composition of magnetic particles. The effect of magnetic particle sizes on the microstructure and magnetic properties of the hot-deformed anisotropic magnet was investigated. Anisotropic hot-deformed magnets produced from the maximum particle size of 200-350 μm have the highest magnetic properties of Br = 1.465 T, Hcj = 1,157 kA.m-1, （Bn）max = 425 kJ.m-3.

Magnetic properties enhancement of hot-deformed NdFeB magnets by two different methods of CeNdCu diffusion

Two different ways were used to control the distribution of cerium for the enhancement of coercivity.One was by coating CeNdCu in the prepared magnet and annealing to make CeNdCu diffuse into the grain boundary to increase the coercivity,the other was by mixing CeNdCu with initial magnetic powders and then preparing the hot-deformed magnet.The SEM-EDS result indicates that cerium diffuses more easily into the main phase by the mixing way,while cerium is mainly distributed in the grain boundary via the coating way.The heat-treatment process may be one of the dominant influencing factors for the distribution of Ce,Multi-steps heat treatment in the mixing way,consisting of hot-pressing,hot-deforming and post heat process,easily introduces Ce into the main phase Nd2 Fe14B,which forms the Ce2 Fe14B shell resulting in the decrease of HA.But the coating way can ensure uniform dispersion of Ce in the grain boundary,which leads to the high coercivity.

Effect of heterogeneous microstructure on magnetization reversal mechanism of hot-deformed Nd-Fe-B magnets

The hot-deformed(HD) Nd-Fe-B magnets show heterogeneous microstructure composed of coarse and fine grain regions. It is significant to fully understand the influence of this complex microstructure on the magnetization reversal process which can give the guidance for the enhancement of the magnetic properties. In this paper, the heterogeneous microstructure of the(HD) Nd-Fe-B magnets were characterized from the morphology, size, macro-texture and micro-structure. In addition, the magnetization reversal process of the HD Nd-Fe-B magnets was systematically analyzed by magnetic measurement, insitu domain evolution observation and micromagnetic simulation. The results indicate that the HD NdFe-B magnets mainly consist of fine grain regions(FGRs) and coarse grain regions(CGRs). The FGRs show plate-like grains with fine grain size and strong c-axis texture, while the CGRs show equiaxial grains with large grain size and weak c-axis texture. In particular, it is worth noting that the texture in homogeneity exists not only between FGRs and CGRs, but also inside both the FGRs and CGRs. The dominant coercivity mechanism of the HD Nd-Fe-B magnets is domain wall pinning. Also, the experimental analysis shows that the reverse domain is formed and expanded in the CGRs at low reverse applied field, while the reverse domain occurs in the FGRs at higher reverse applied field. The micromagnetic simulation results also confirm the above magnetization reversal process. In addition, micromagnetic simulation results also show that the orientation of the grains also affects the pinning strength, besides the grain size.

Effect of Pr-Ga dual-alloys diffusion on magnetic properties and thermal stability of hot-deformed PrNd-Fe-B magnets

To investigate the influence of the addition of Pr-Ga alloys on magnetic properties and morphology of materials,the hot-deformed PrNd-Fe-B magnets were prepared by the addition of Pr-Ga alloys using a dual-alloys diffusion.The room-temperature coercivity of the hot-deformed PrNd-Fe-B magnets increases substantially from 1.68 to 2.34 T,while the remanence decreases from 1.42 to 1.24 T,by the addition of 5 wt%Pr-Ga alloys.Moreover,the thermal stability of coercivity improves from-0.46%/℃to-0.42%/℃.Two types of grain boundary phases(PrNd-rich and PrNd-Ga-rich)are generated at grain boundaries by microstructural analysis,resulting in the decrease of Fe element concentration from more than 60%to about 10%at grain boundaries.The decrease of ferromagnetic element concentration at grain boundaries and the refinement of grain are considered to be the main reasons for the improvement of coercivity and thermal stability.

Analysis on deformation and texture formation mechanism of hot-deformed Nd-Fe-B magnets based on heterogeneous structure evolution

In this paper, microstructure, micromagnetic structure, texture, together with magnetic properties of the hot-deformed(HD) Nd-Fe-B magnets were systematically studied to understand the deformation process and the formation mechanism of c-axis texture. The results show that the platelet grains are formed in the fine-grain regions at the initial stage of the deformation. As the amount of deformation increases, the proportion of platelet grains increases and arranges gradually, causing the formation of c-axis texture, till the grain merging occurres when the deformation is excessive. It should be noted that the rare earth-rich phase in the fine-grained region slowly diffuses to the coarse-grained region where only grain growth can be observed during deformation. The deformation mechanism and formation of c-axis texture in HD Nd-Fe-B magnets can be deduced to be accomplished by the processes of dissolution-precipitation diffusion, grain rotation and grain arrangement, based on the characterization of microstructure and texture evolution. Also, approaches to optimize the preparation process and magnetic properties of the hot-deformed Nd-Fe-B magnets were discussed.

Preparation and properties of hot-deformed magnets processed from nanocrystalline/amorphous Nd-Fe-B powders

The hot-deformed magnets processed from nanocrystalline/amorphous Nd-Fe-B powders were preparedunderdifferenthot-pressingtemperatures(600-750℃,at intervals of 25℃)by the self-made hotpressing equipment.The microstructure and magnetic properties of hot-deformed magnets prepared at different temperatures were also investigated.When the temperature is above 650℃,the density of magnet reaches 7.5 g·cm^(-3).The optimum magnetic properties of magnetic induction intensity of B_(r)=1.3 T,optimum energy product of(BH)_(max)=282.5 kJ·m^(-3),intrinsiccoercivityof H_(cj)=1130.0 kA·m-1 of hot-deformed magnets are obtained at hot-pressing temperature of 650℃.X-ray diffractometer pattern shows that the(00 L)texture has been obtained.For the microstructural characteristic,on the one hand,the good magnetic performance is attributed to the fine platelet-like grains with an average length of 410-440 nm at the hot-pressing temperature range from625 to 675℃.On the other hand,the unaligned coarse grains are observed in all the samples.And the areal fraction of those is gradually increasing with the rise of the hot-pressing temperature,which tends to deteriorate the magnetic properties.The composition map shows the accumulation of Nd/Pr-rich phase in the coarse grains’region.

Sandwiched structure of hot-deformed Nd-Fe-B permanent magnets processed by Nd-Cu eutectic alloys diffusion

A series of sandwiched structures with different near-surface mass fractions x(x=3 wt%,4 wt%,5 wt%)was employed to develop high-coercivity hot-deformed Nd-Fe-B magnets by the addition of 2 wt%Nd-Cu eutectic alloys via adjusting the middle thickness and near-surface thickness.The designed magnet with a pronounced composite structure shows a 23% increase in coercivity with a 6% loss of remanence by adjusting the sandwiched structure at 4 wt% Nd-Cu eutectic alloys in the near-surface regions.The results indicate that the near-surface Nd-Cu-rich "shell" structure can effectively suppress the magnetization reversal of overall magnets,enhancing the coercivity.With the help of loading stress,Nd-Cu liquid enriched at the near-surface regions of the sample is infiltrated into the Nd-Cu-lean middle region,resulting in a concentration gradient.Microstructure characterizations further demonstrate that the infiltrated Nd-Cu eutectic plays a critical role in inhibiting grain growth and intergranular magnetic interaction.The optimized microstructure features suppress the reversed magnetization process,which makes a positive contribution to coercivity.

Coercivity enhancement of Ce-containing hot-deformed magnets by grain boundary diffusion of DyF_(3)

The samples with full density were prepared by hot pressing the the melt-spun powders mixed with DyF_(3)powders of different mass fractions followed by hot-deformation process.The magnetic properties and temperature dependence of coercivity were obtained by BH tracer and VSM,respectively.The microstructure were analyzed by scanning electron microscopy(SEM)and transmission electron microscopy(TEM).The coercivity of Ce-containing hot-deformed magnets is increased from 1.41 to 1.95 T by grain boundary diffusion of 3 wt%DyF_(3),and is further enhanced to 2.05 T after annealing treatment.The thermal stability of coercivity and remanence is improved.The annealing condition in this work crucially plays a role in thickening the grain boundary phase.Microstructure analysis reveals that the continuous and thick grain boundary phase formed after DyF_(3)diffusion can weaken the magnetic coupling between grains,and suppress the platelet shaped grain size and the aspect ratio.The Dycontaining shell structure formed by the partial diffusion of Dy into the main phase can increase the magnetic anisotropy field,which is the main reason for the coercivity improvement.After optimizing the structure by DyF_(3)diffusion,the"dendritic-like"reverse domain is transformed into the"dot scatteredlike"reverse domain.

Effect of crushing methods on morphology and magnetic properties of anisotropic NdFeB powders

Crushing is a critical factor for the anisotropic Nd Fe B powders with high magnetic properties. However, the traditional crushing methods of disk-milling（DM） or impact crushing（IC）, are difficult to obtain high-performance powders. Herein, a new method of preparing anisotropic powders with high performance was reported, which was through crushing the hot-deformed magnets perpendicular to c-axis direction（shear crushing, SC）. The microstructure and alignment of the magnets were examined by scanning electron microscopy（SEM） and X-ray diffraction（XRD）, respectively. The results indicated that the cracks mainly extended along the Nd-rich grain boundary phase and/or the binding interface of ribbons. It not only could protect the magnetic phase from being damaged, but also could keep the grains integrated. Therefore, shear crushing was an effective method for the preparation of highperformance anisotropic powders and then to fabricate the bonded magnets with Br=9.0 kGs, Hci=10.48 kOe and（BH）max=17.7 MGOe.