Effects of terbium sulfide addition on magnetic properties,microstructure and thermal stability of sintered Nd-Fe--B magnets

To increase coercivity and thermal stability of sintered Nd–Fe–B magnets for high-temperature applications, a novel terbium sulfide powder is added into（Pr（0.25）Nd（0.75））（30.6）Cu（0.15）Fe（bal）B1（wt.%） basic magnets. The effects of the addition of terbium sulfide on magnetic properties, microstructure, and thermal stability of sintered Nd–Fe–B magnets are investigated.The experimental results show that by adding 3 wt.% Tb2S3, the coercivity of the magnet is remarkably increased by about 54% without a considerable reduction in remanence and maximum energy product. By means of the electron probe microanalyzer（EPMA） technology, it is observed that Tb is mainly present in the outer region of 2：14：1 matrix grains and forms a well-developed Tb-shell phase, resulting in enhancement of HA, which accounts for the coercivity enhancement.Moreover, compared with Tb2S3-free magnets, the reversible temperature coefficients of remanence（α） and coercivity（β） and the irreversible flux loss of magnetic flow（hirr） values of Tb2S3-added magnets are improved, indicating that the thermal stability of the magnets is also effectively improved.

Effects of post-sinter annealing on microstructure and magnetic properties of Nd–Fe–B sintered magnets with Nd–Ga intergranular addition

We investigate the effects of post-sinter annealing on the microstructure and magnetic properties in B-lean Nd–Fe–B sintered magnets with different quantities of Nd–Ga intergranular additions. The magnet with fewer Nd–Ga additions can enhance 0.2 T in coercivity, with its remanences nearly unchanged after annealing. With the further increase of the Nd–Ga addition, the annealing process leads coercivity to increase 0.4 T, accompanied by a slight decrease of remanence. With the Nd–Ga addition further increasing and after annealing, however, the increase of coercivity is basically constant and the change of remanence is reduced. Microstructure observation indicates that the matrix grains are covered by continuous thin grain boundary phase in the magnets with an appropriate Nd–Ga concentration after the annealing process. However, the exceeding Nd–Ga addition brings out notable segregation of grain boundary phase, and prior formation of part RE6 Fe13 Ga phase in the sintered magnet. This prior formation results in a weaker change of remanence after the annealing process.Therefore, the diverse changes of magnetic properties with different Nd–Ga concentrations are based on the respective evolution of grain boundary after the annealing process.

Phase constitution and microstructure of Ce–Fe–B strip-casting alloy

The strip-casting technique plays an important role in fabricating high coercivity sintered magnet. In this paper, we investigate the phase constitution and the microstructure of rapidly solidified Ce-Fe-B alloy fabricated by strip-casting. We find that the Ce2FelgB phase coexists with Fe, Fe2B, and CeFe2 phases in the Ce-Fe-B strips. The eutectic stucture consisting of Fe and Fe2B is encased in Ce2Fe14B grains, which is blocked by the CeFe2 grains at triple junctions, indicating that the microstructure of Ce-Fe-B strip is characteristic of a peritectic solidification. Thermal analysis indicates that the large supercooling of Ce2Fe14B results in the residual Fe and Fe2B. The microstructural optimization in Ce-Fe-B strips without Fe and Fe2B could be achieved by a heat treatment of 1000 ℃.

Improvement in coercivity,thermal stability,and corrosion resistance of sintered Nd-Fe-B magnets with Dy_(80)Ga_(20) intergranular addition

To investigate the coercivity,corrosion resistance,and thermal stability of Nd-Fe-B magnets,their properties were investigated at room and high temperature before and after doping with Dy（80）Ga（20）（at.%） powder.The coercivity of the magnets increased from the undoped value of 12.72 kOe to a doped value of 21.44 kOe.A micro-structural analysis indicates that a well-developed core-shell structure forms in the magnets doped with Dy（80）Ga（20） powder.The improvement in magnetic properties is believed to be related to the refined and uniform matrix grains,continuous grain boundaries,and a hardened（Nd,Dy）2Fe（14）B shell surrounding the matrix grains.Additionally,the doped magnets exhibit an obvious improvement in thermal stability.For the magnets with added Dy（80）Ga（20） powder,the temperature coefficients of remanence（α） and coercivity（β） increased to-0.106%℃-（-1） and-0.60%℃-（-1） over the range 20-100 ℃,compared to temperature coefficients of-0.117%℃-（-1）（α） and-0.74%℃-（-1）（β） in the regular magnets without Dy（80）Ga（20） powder.The irreversible loss of magnetic flux（Hirr） was investigated at different temperatures.After being exposed to 150 ℃ for 2 h,the Hirr of magnets with 4 wt.%Dy（80）Ga（20） decreased by -95%compared to that of the undoped magnets.The enhanced temperature coefficients and Hirr indicate improved thermal stability in the doped Nd-Fe-B magnets.The intergranular addition of Dy（80）Ga（20） also improved the corrosion resistance of the magnets because of the enhanced intergranular phase.In a corrosive atmosphere for 96 h,the mass loss of the sintered magnets with 4 wt.%Dy（80）Ga（20） was 2.68 mg/cm-2,less than 10%of that suffered by the undoped magnets（28.1 mg/cm-2）.

High-precision nuclear magnetic resonance probe suitable for in situ studies of high-temperature metallic melts

High-temperature nuclear magnetic resonance(NMR)has proven to be very useful for detecting the temperatureinduced structural evolution and dynamics in melts.However,the sensitivity and precision of high-temperature NMR probes are limited.Here we report a sensitive and stable high-temperature NMR probe based on laser-heating,suitable for in situ studies of metallic melts,which can work stably at the temperature of up to 2000 K.In our design,a well-designed optical path and the use of a water-cooled copper radio-frequency(RF)coil significantly optimize the signal-to-noise ratio(S/NR)at high temperatures.Additionally,a precise temperature controlling system with an error of less than±1 K has been designed.After temperature calibration,the temperature measurement error is controlled within±2 K.As a performance testing,^(27)Al NMR spectra are measured in Zr-based metallic glass-forming liquid in situ.Results show that the S/NR reaches 45 within 90 s even when the sample's temperature is up to 1500 K and that the isothermal signal drift is better than0.001 ppm per hour.This high-temperature NMR probe can be used to clarify some highly debated issues about metallic liquids,such as glass transition and liquid-liquid transition.

Core structure and Peierls stress of the 90°dislocation and the 60°dislocation in aluminum investigated by the fully discrete Peierls model

The core structure,Peierls stress and core energy,etc.are comprehensively investigated for the 90°dislocation and the 60°dislocation in metal aluminum using the fully discrete Peierls model,and in particular thermal effects are included for temperature range 0≤T≤900 K.For the 90°dislocation,the core clearly dissociates into two partial dislocations with the separating distance D~12?,and the Peierls stress is very smallσp<1 k Pa.The nearly vanishing Peierls stress results from the large characteristic width and a small step length of the 90°dislocation.The 60°dislocation dissociates into 30°and 90°partial dislocations with the separating distance D~11A.The Peierls stress of the 60°dislocation grows up from1 MPa to 2 MPa as the temperature increases from 0 K to 900 K.Temperature influence on the core structures is weak for both the 90°dislocation and the 60°dislocation.The core structures theoretically predicted at T=0 K are also confirmed by the first principle simulations.

Anomalous microstructure and magnetocaloric properties in off-stoichiometric La–Fe–Si and its hydride

In the present work we reported the phase formation, microstructure, magnetocaloric effect and hydrogenation behavior of La-rich La1.7Fe11.6Si1.4alloy. In this off-stoichiometric La（Fe,Si）13alloy, the Na Zn13-type La（Fe,Si）13matrix phase shows faceted grains, with the Cr5B3-type La5Si3 used as the secondary phase distributed intergranularly. Such a peculiar morphology quickly forms upon one day annealing. In La1.7Fe11.6Si1.4alloy, we have observed a significant field dependence of magnetostructural transition temperature（～ 6.3 K/T）, resulting in a large and table-like entropy change（△S～ 18 J/kg·K in 2 T） over a broad temperature range（～ 10 K）. Upon hydrogenation, the maximum value of △S keeps almost unchanged, while the Curie temperature increases up to 350 K. These results indicate that the investigated offstoichiometric La（Fe,Si）13alloy is a promising magnetic material for magnetic refrigerators.

Electric modulation of anisotropic magnetoresistance in Pt/HfO_(2-x)/NiO_(y)/Ni heterojunctions

Electric field control of magnetism through nanoionics has attracted tremendous attention owing to its high efficiency and low power consumption.In solid-state dielectrics,an electric field drives the redistribution of ions to create onedimensional magnetic conductive nanostructures,enabling the realization of intriguing magnetoresistance(MR)effects.Here,we explored the electric-controlled nickel and oxygen ion migration in Pt/HfO_(2-x)/NiO_(y)/Ni heterojunctions for MR modulation.By adjusting the voltage polarity and amplitude,the magnetic conductive filaments with mixed nickel and oxygen vacancy are constructed.This results in the reduction of device resistance by~10^(3)folds,and leads to an intriguing partial asymmetric MR effect.We show that the difference of the device resistance under positive and negative saturation magnetic fields exhibits good linear dependence on the magnetic field angle,which can be used for magnetic field direction detection.Our study suggests the potential of electrically controlled ion migration in creating novel magnetic nanostructures for sensor applications.

Electronic structure of cuprate-nickelate infinite-layer heterostructure

The discovery of superconductivity in Sr/Ca-doped infinite-layer nickelates Nd(La)NiO_(2)thin films inspired extensive experimental and theoretical research.However,research on the possibilities of enhanced critical temperature by interface heterostructure is still lacking.Due to the similarities of the crystal structure and band structure of infinite-layer nickelate La NiO_(2)and cuprate CaCuO_(2),we investigate the crystal,electronic and magnetic properties of La NiO_(2):CaCuO_(2)heterostructure using density functional theory and dynamical mean-field theory.Our theoretical results demonstrate that,even a very weak inter-layer z-direction bond is formed,an intrinsic charge transfer between Cu-3d_(x^(2)-y^(2))and Ni-3d_((x^(2)-y^(2)))orbitals is obtained.The weak interlayer hopping between Cu and Ni leaves a parallel band contributed by Ni/Cu-3d_((x^(2)-y^(2)))orbitals near the Fermi energy.Such an infinite-layer heterostructure with negligible interlayer interaction and robust charge transfer opens a new way for interface engineering and nickelate superconductors.

Novel CoFeAlMn high-entropy alloys with excellentsoft magnetic properties and high thermal stability

High-entropy alloys(HEAs),which are composed of 3d transition metals such as Fe,Co,and Ni,exhibit an exceptional combination of magnetic and other properties;however,the addition of non-ferromagnetic elements always negatively affects the saturation magnetization strength(M s).Co_(4)Fe_(2)Al_(x)Mn_(y) alloys were designed and investigated in this study to develop a novel HEA with excellent soft magnetic properties.The Co_(4)Fe_(2)Al_(1.5)Mn_(1.5) HEA possesses the highest M s of 161.3 emu g^(-1) thus far reported for magnetic HEAs,a low coercivity of 1.9 Oe,a high electrical resistivity of 173μΩ cm,a superior thermal stability up to 600℃,which originates from the novel microstructure of B2 nanoparticles distributed in a DO_(3) matrix phase,and the crucial transition of Mn from antiferromagnetism to ferromagnetism with the assistance of Al.The Co_(4)Fe_(2_)Al_(1.5)Mn_(1.5) HEA was selected to produce micron-sized powder and soft magnetic powder cores(SMPCs)for application in the exploration field.The SMPCs exhibit a high stable effective perme-ability of 35.9 up to 1 MHz,low core loss of 38.1 mW cm^(-3)(@100 kHz,20 mT),and an excellent direct current(DC)bias performance of 87.7%at 100 Oe.This study paves the way for the development of soft magnetic HEAs with promising applications as magnetic functional materials.

Effect of aluminum on microstructure and magnetic properties of sintered Nd-Fe-B magnets processed by grain boundary diffusion of Tb-Al

The grain boundary diffusion process(GBDP)of Tb can improve the coercivity of sintered Nd-Fe-B magnets.In this study,the effect of AI on the diffusion of Tb in the GBDP was investigated.The content of diffused Tb-Al was precisely controlled by adjusting the magnetron sputtering process.The Tb equivalent of Al was also studied.Results show that AI promotes the diffusion of Tb deeper into the magnet,reducing the thickness of the shell in the core-shell structure.This study is helpful for further developing the process,reducing the consumption of heavy rare earth elements(Tb),and improving the coercivity of sintered Nd-Fe-B magnets.

Enhanced energy storage behaviors in free-standing antiferroelectric Pb(Zr_(0.95)Ti_(0.05))O_3 thin membranes

Free-standing antiferroelectric Pb（Zr0.95Ti0.05O3（PZT（95/5）） thin film is fabricated on 200-nm-thick Pt foil by using pulsed laser deposition.X-ray diffraction patterns indicate that free-standing PZT（95/5） film possesses an α-axis preferred orientation.The critical electric field for the 300-nm-thick free-standing PZT（95/5） film transiting from antiferroelectric to ferroelectric phases is increased to 770 kV/cm,but its saturation polarization remains almost unchanged as compared with that of the substrate-clamped PZT（95/5） film.The energy storage density and energy efficiency of the substrate-clamped PZT（95/5） film are 6.49 J/cm^3 and 54.5%,respectively.In contrast,after removing the substrate,the energy storage density and energy efficiency of the free-standing PZT（95/5） film are enhanced up to 17.45 J/cm^3 and 67.9%,respectively.

Local leakage current behaviours of BiFeO_3 films

The leakage current behaviours of polycrystalline BiFeO3 thin films are investigated by using both conductive atomic force microscopy and current-voltage characteristic measurements. The local charge transport pathways are found to be located mainly at the grain boundaries of the films. The leakage current density can be tuned by changing the post-annealing temperature, the annealing time, the bias voltage and the light illumination, which can be used to improve the performances of the ferroelectric devices based on the BiFeOa films. A possible leakage mechanism is proposed to interpret the charge transports in the polycrystalline BiFeO3 films.

Effect of thermal deformation on giant magnetoresistance of flexible spin valves grown on polyvinylidene fluoride membranes

We fabricated flexible spin valves on polyvinylidene fluoride（PVDF） membranes and investigated the influence of thermal deformation of substrates on the giant magnetoresistance（GMR） behaviors. The large magnetostrictive Fe_（81）Ga_（19）（Fe Ga） alloy and the low magnetostrictive Fe_（19）Ni_（81）（Fe Ni） alloy were selected as the free and pinned ferromagnetic layers.In addition, the exchange bias（EB） of the pinned layer was set along the different thermal deformation axes α_（31） or α_（32） of PVDF. The GMR ratio of the reference spin valves grown on Si intrinsically increases with lowering temperature due to an enhancement of spontaneous magnetization. For flexible spin valves, when decreasing temperature, the anisotropic thermal deformation of PVDF produces a uniaxial anisotropy along the α_（32） direction, which changes the distribution of magnetic domains. As a result, the GMR ratio at low temperature for spin valves with EB α_（32）becomes close to that on Si, but for spin valves with EB α_（31）is far away from that on Si. This thermal effect on GMR behaviors is more significant when using magnetostrictive Fe Ga as the free layer.

Improved photovoltaic effects in Mn-doped BiFeO3 ferroelectric thin films through band gap engineering

As a low-bandgap ferroelectric material, BiFeO3 has gained wide attention for the potential photovoltaic applications,since its photovoltaic effect in visible light range was reported in 2009. In the present work, Bi（Fe, Mn）O3thin films are fabricated by pulsed laser deposition method, and the effects of Mn doping on the microstructure, optical, leakage,ferroelectric and photovoltaic characteristics of Bi（Fe, Mn）O3 thin films are systematically investigated. The x-ray diffraction data indicate that Bi（Fe, Mn）O3 thin films each have a rhombohedrally distorted perovskite structure. From the light absorption results, it follows that the band gap of Bi（Fe, Mn）O3 thin films can be tuned by doping different amounts of Mn content. More importantly, photovoltaic measurement demonstrates that the short-circuit photocurrent density and the open-circuit voltage can both be remarkably improved through doping an appropriate amount of Mn content, leading to the fascinating fact that the maximum power output of ITO/BiFe（0.7）Mn（0.3）O3/Nb-STO capacitor is about 175 times higher than that of ITO/BiFeO3/Nb-STO capacitor. The improvement of photovoltaic response in Bi（Fe, Mn）O3 thin film can be reasonably explained as being due to absorbing more visible light through bandgap engineering and maintaining the ferroelectric property at the same time.

The magnetization reversal behaviour for SmCo_(6.8)Zr_(0.2) and SmCo_(6.8)Zr_(0.2)/α-(Fe,Co) nanocrystalline magnets at low temperature

This paper reports that the SmCo6.8Zr0.2 nanocrystalline permanent magnets and SmCo6.8Zr0.2/a-（Fe,Co） nanocomposite permanent magnets are successfully produced by mechanical alloying and subsequently annealing at 700℃ for 10 minutes. The x-ray diffraction results show that the phase structure of SmCo6.8Zr0.2 nanocrystalline permanent magnets is composed of SmCo7 phase and SmCo6.8Zr0.2/a-（Fe,Co） nanocomposite permanent magnets is composed of SmCo7 and a-（Fe,Co） phases. The mechanism of magnetization reversal is mainly controlled by inhomogeneous domain wall pinning in SmCo6.8Zr0.2 and SmCo6.8Zr0.2/a-（Fe,Co） magnets. The inter-grain exchange interaction at low temperature is investigated, which shows that the inter-grain exchange interaction of SmCo6.8Zr0.2/a-（Fe,Co） magnets increases greatly by the decrease of the measured temperature. According to Amirr-H/Hcj, Amrev-H/Hcj and Xirr-H/Hcj curves at room temperature and 100 K, the changes of irreversible and reversible magnetization behaviours of SmCo6.8Zr0.2 and SmCo6.8Zr0.2/a-（Fe,Co） magnets with the decreasing temperature are analysed in detail. The magnetic viscosity and the activation volume of SmCo6.8Zr0.2 and SmCo6.8Zr0.2/a-（Fe,Co） magnets at different temperatures are also studied.

Fine-grained NdFeB magnets prepared by low temperature pre-sintering and subsequent hot pressing

Fine-grained Nd10.79Pr2.8Al0.4B7.72Fe78.29 magnets were prepared by low temperature pre-sintering and subsequent hot pressing. The grain size of the magnets is just about 1–3 μm because the low sintering temperature results in no grain growth. The orientation degree, microstructure, and magnetic properties were studied. Some grains＇ easy axes deviate from the orientation direction, possibly due to grain rotation during the hot pressing. By subsequent annealing, the magnetic properties were significantly enhanced. Especially, the squareness of the demagnetization curve was improved greatly.The enhancement of coercivity by annealing can be explained by an improvement of both grain boundaries and magnetic isolation, which decouples the exchange interaction between neighboring grains.

Small activation entropy bestows high-stability of nanoconfined D-mannitol

It has been a long-standing puzzling problem that some glasses exhibit higher glass transition temperatures(denoting high stability)but lower activation energy for relaxations(denoting low stability).In this paper,the relaxation kinetics of the nanoconfined D-mannitol(DM)glass was studied systematically using a high-precision and high-rate nanocalorimeter.The nanoconfined DM exhibits enhanced thermal stability compared to the free DM.For example,the critical cooling rate for glass formation decreases from 200 K/s to below 1 K/s;the Tg increases by about 20 K–50 K.The relaxation kinetics is analyzed based on the absolute reaction rate theory.It is found that,even though the activation energy E^(*)decreases,the activation entropy S^(*)decreases much more for the nanoconfined glass that yields a large activation free energy G^(*)and higher thermal stability.These results suggest that the activation entropy may provide new insights in understanding the abnormal kinetics of nanoconfined glassy systems.

Investigation of magnetization reversal process in pinned CoFeB thin film by in-situ Lorentz TEM

Exchange bias effect has been widely employed for various magnetic devices.The experimentally reported magnitude of exchange bias field is often smaller than that predicted theoretically,which is considered to be due to the partly pinned spins of ferromagnetic layer by antiferromagnetic layer.However,mapping the distribution of pinned spins is challenging.In this work,we directly image the reverse domain nucleation and domain wall movement process in the exchange biased Co Fe B/Ir Mn bilayers by Lorentz transmission electron microscopy.From the in-situ experiments,we obtain the distribution mapping of the pinning strength,showing that only 1/6 of the ferromagnetic layer at the interface is strongly pinned by the antiferromagnetic layer.Our results prove the existence of an inhomogeneous pinning effect in exchange bias systems.

Influence of RE-rich phase distribution in initial alloy on anisotropy of HDDR powders

The influence of the RE-rich phase distribution in the precursor alloys on the anisotropy of the hydrogenation disproportionation desorption recombination（HDDR） processed powders is investigated. The homogenized ingot alloy and the as-cast strip casting（SC） alloy with a uniform RE-rich grain boundary phase lead to high anisotropy of the refined powders,acquiring degrees of alignment（DOA） of 0.62 and 0.54, respectively. The RE-rich phase aggregation results in a deteriorated DOA of the powders due to the drastic disproportionation rate, while a thin and uniform RE-rich phase distribution is beneficial for DOA. A reaction model of the initial particle microstructure is proposed for optimizing the HDDR powder anisotropy.