Effect of niobium substitution on microstructures and thermal stability of TbCu7-type Sm–Fe–N magnets

This paper reports crystal structures, magnetic properties and thermal stability of TbCu7-type Sm_(8.5)Fe_((85.8-x)Co_(4.5)Zr_(1.2)Nb_x(x = 0-1.8) melt-spun compounds and their nitrides, investigated by means of X-ray diffraction, vibrating sample magnetometer, flux meter and transmission electron microscope. It is found that the lattice parameter ratio c/a of TbCu_7-type crystal structure increases with Nb substitution, which indicates that the Nb can increase the stability of the metastable phase in the Sm-Fe ribbons. Nb substitution impedes the formation of magnetic soft phase a-Fe in which reversed domains initially form during the magnetization reversal process. Meanwhile, Nb substitution refines grains and leads to homogeneous micro structure with augmented grain boundaries. Thus the exchange coupling pining field is enhanced and irreversible domain wall propagation gets suppressed. As a result, the magnetic properties are improved and the irreversible flux loss of magnets is notably decreased. A maximum value 771.7 kA/m of the intrinsic coercivity H_(cj) is achieved in the 1.2 at% substituted samples.The irreversible flux loss for 2 h exposure at 120 ℃ declines from 8.26% for Nb-free magnets to 6.32% for magnets with 1.2 at% Nb substitution.     

Crystal structure and hard magnetic properties of TbCu_7-type Sm_(0.98)Fe_(9.02–x)Ga_x nitrides

The compound Sm0.98Fe9.02–xGaxNδ(x=0, 0.25, 0.5, 0.75, 1) were prepared by melt-spun method and subsequent annealing and nitriding. The Rietveld analysis showed that the lattice expansion played an important role in improving the Curie temperature. An obvious development of the Curie temperature was obtained with the increased Ga content from x=0–1(ΔTc=90 oC). The optimum coercivity of nitrides was obtained at x=0.25 with the value Hcj=652 kA/m(8.15 kOe) after annealing, which corresponded to a reasonable distribution of grain sizes of both TbCu7-type SmFe9Nδ and α-Fe. However, an excess of Ga doping might lead to an abnormal growth of α-Fe, which in turn deteriorated the magnetic properties. It was concluded that a moderate Ga content was very effective in raising the coercivity and Curie temperament in the TbCu7-type Sm-Fe-N.     

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.     

Novel synthesis of single-crystalline TbCu7-type Sm–Fe powder by low-temperature reduction-diffusion process using molten salt

In this study, molten salt was used as a solvent for calcium (Ca) to let a reduction-diffusion (R-D) reaction occur below the melting point of Ca (1115 K), which is the lower limit temperature of the conventional R-D process. When the R-D reaction is conducted below 923 K with LiCl molten salt, submicron-sized TbCu₇-type Sm–Fe powder is formed. The c/a ratio of the powder estimated by a synchrotron X-ray diffraction pattern is 0.8456, which is consistent with the Sm_0.67Fe_5.667(SmFe_8.5) phase. An electron backscatter diffraction analysis reveals that single-crystalline TbCu₇-type SmFe_8.5 powder was synthesized for the first time.     

Relationship between controllable preparation and microstructure of NdFeB sintered magnets

The double hard magnetic phase magnets with nominal compositions of Nd_30–xDy_xFe₆₉B₁(x=2, and 4) (wt.%) were prepared. The magnetic properties of the magnets were measured with a NIM-2000H hysteresigraph. The crystalline structures of the magnets were identified by X-ray diffraction (XRD). The Rietveld refinement was carried out using the FULLPROF software. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses were carried out in order to investigate the microstructure of the magnets. It showed that the magnets consisted mainly of Nd₂Fe₁₄B phase, and some Nd-rich phase. Two types of matrix-phase grains in dark grey and light grey were found in the magnets with x=2 and 4. The Dy content was obviously different in the two types of grains, which proved that the double hard magnetic phases (Dy-rich and Dy-lean phases) coexisted in the magnet. It revealed that the Nd-rich phases in junction regions had fcc structure, with the unit cell parameter of about 0.52–0.56 nm. The weak superlattice spots were found in the SAD patterns of the junction Nd-rich phases with large scale. The double hard magnetic phase structure seemed to improve the magnetic properties of NdFeB magnets with high coercivity, while decrease the consumption of Dy element, compared with the single alloy magnet.     

Synthesis and structural characterization of nanocrystalline Ni<Subscript>50</Subscript>Al<Subscript>50 − <Emphasis Type="Italic">x</Emphasis></Subscript>Mo<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> intermetallic compound prepared by mechanical alloying

Nanocrystalline Ni₅₀Al_{50 ? x} Mo _x (x = 0, 0.5, 1, 2.5, and 5) intermetallic powders were synthesized by mechanical alloying (MA). Microstructural characterization and structural changes of powder particles during mechanical alloying were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results confirmed that the synthesis behavior of NiAl intermetallic depends on the Mo content and milling time. The SEM micrograph outcomes confirmed the specimen with longer milling time includes finer and more homogenous particles with attention to the ones with lesser milling time. Mo enhance has a considerable effect on the lowering of crystallite size. The TEM image showed that the Ni₅₀Al₄₅Mo₅ nano-particles were less than 10 nm.     

Effect of cobalt substitution on structure and magnetic properties of Nd_(0.4)Zr_(0.6)Fe_(10-x)Co_xSi_2(x =0-3) alloys and their ribbons

This study reports the stabilization of the RFe_(12)-type based compounds where part of R and Fe are substituted with Zr and Co and Si, respectively, in order to examine whether these rare-earth-lean materials are suitable for applications as permanent magnets. Structural and magnetic characterization of the family of alloys with the general formula Nd_(0.4) Zr_(0.6) Fe_(10-x)Co_xS_i2(x = 0 -3) and their melt-spun ribbons were carried out using X-ray diffraction and M€ossbauer spectroscopy. The ThMn_(12)-type structure is obtained for all samples as the majority phase with a minority a-Fe(CoSi) phase(less than 5 wt%) as it was estimated by XRD for x = 1 and 2. The Curie temperature increases linearly with Co substitution from 561 K for x = 0 to 712 K for x = 3. The saturation magnetization decreases slightly from 130.5(x =1)to 129.1 A·m~2/kg(x=3), while the anisotropy field is following the same trend.     

Magnetic properties and microstructure of Fe_(69.5-x)Nd_7B_(21)Nb_(2.5)Ga_x(x=0-1)alloys

The Fe_(69.5-x)Nd_7 B_(21)Nb_(2.5)Ga_x(x = 0-1)permanent magnets in the form of rods were prepared by annealing the bulk amorphous alloys.The magnetic properties,phase evolution and microstructure of the alloys were investigated systematically.It is found that the glass forming ability(GFA), microstructure and magnetic properties are sensitive to Ga content for Fe_(69.5-x)Nd_7 B_(21)Nb_(2.5)Ga_x(x = 0-1)bulk alloys.The annealed alloys are mainly composed of soft α-Fe,hard Nd_2 Fe_(14)B and nonmagnetic Nd_(1.1)Fe_4 B_4 phases.When x = 0.3,the optimally annealed magnets exhibit magnetic properties of the remanence Br = 0.63 T,intrinsic coercivity H_(cj) = 368.68 kA/m and maximum energy product(BH)_(max) = 33.73 kJ/m~3.Furthermore,magnetic field heat treatment at the temperature close to Curie temperature of Nd_2 Fe_(14)B phase was applied to the annealed Fe_(69.2)Nd_7 B_(21)Nb_(2.5)Ga_(0.3) magnet.The results of X-ray diffraction(XRD)and transmission electron microscopy(TEM)indicate that the magnetic field heat treatment can be beneficial for the precipitation of α-Fe.Thus,the B_r,H_(cj) and(BH)_(max) are enhanced by 8.7%,6.3% and 16.3%,respectively.     

Formation of metastable phases of Ni-C

Mechanical alloying (MA) of nickel and graphite powders was performed in the composition range Ni_1-xC_x (x = 0.10 to 0.90) by use of a conventional ball mill. The structure of me-chanically alloyed samples was examined by X-ray diffraction, transmission electron micros-copy (TEM), scanning electron microscopy (SEM), and differential scanning calorimetry. A remarkable supersaturation of carbon in face-centered cubic (fcc) nickel phase was observed. A metastable phase Ni₃C was formed by a prolonged MA treatment. For the purpose of com-parative study, MA of cobalt and graphite powders was also performed in composition Co_1-xC_x (x = 0.10, 0.15, and 0.30). The supersaturation of carbon in fcc cobalt and formation of a metastable carbide Co₃C were confirmed.     

Characterization of α-Fe-Free Heteroepitaxial NdFe12−x Ti x Thin-Film Materials with a Novel Cubic Laves Fe2Ti Phase

Thin films with compositions of NdFe₁₂ and NdFe₁₁Ti₁ were fabricated on W-buffered MgO(001) substrates of varying roughness. In this study, X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the films microstructurally, chemically, and crystallographically. This study revealed successful heteroepitaxial synthesis of the tetragonal NdFe₁₂ and NdFe_12−x Ti _x phases in the Ti-free and Ti-containing films, respectively, both with surface-normal c-axis orientation. It also revealed the presence of other phases within the magnetic layer. The NdFe₁₂ films contained many α-Fe particles, which preferentially precipitated at locally rough regions of the W-buffer interface. The NdFe₁₁Ti₁ film showed the ubiquitous presence of an Fe₂Ti phase, which covered most of the buffer thereby preventing the formation of α-Fe. This phase was determined to have a novel Cu₂Mg-type cubic Laves (C15) crystal structure with fourfold interfacial symmetry, good coherency, and a low mismatch with the W-buffer, thus rendering itself as being an ideal interface for the heteroepitaxial synthesis of NdFe_12−x Ti _x crystals. It is proposed that successful application of a cubic Fe₂Ti underlayer on W can contribute to the development of a fabrication strategy for NdFe₁₂ thin films without the presence of soft magnetic α-Fe.

     

Effects of Sm-doping on microstructure,magnetic and microwave absorption properties of BiFeO_3

In this paper,polycrystalline samples of Bi_(1-x)Sm_xFeO~3(x=0,0.05,0.1,0.15) were successfully synthesized by sol-gel method.The effects of Sm concentration on the crystal structure,morphology,chemical states,magnetic properties and microwave absorption performance were studied by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),a vibrating sample magnetometer(VSM) and a Vector network analyzer(VNA),respectively.The results show that the rare earth Sm doping causes the crystal structure to change.When x≤0.1,Bi_(1-x)Sm_xFeO_3 is the distorted rhombohedral structure with space group R3 c.With the increase of Sm doping amount to x=0.15,the phase structure of Bi_(1-x)Sm_xFeO_3 changes from rhombohedral structure to cubic structure with the space group Pm3 m.The particle size decreases with the increase of the Sm doping amount.The analysis results show that Sm doping can effectively reduce the oxygen vacancies and significantly improve its magnetic properties.The results exhibit that moderately doped rare earth Sm element can effectively improve microwave absorption properties of Bi_(1-x)Sm_xFeO_3 powders.When Sm doping amount of x is 0.1,the Bi_(0.9)Sm_(0.1) FeO_3 compound has good microwave absorption performance,and the minimum reflection loss value of Bi_(0.9)Sm_(0.1)FeO_3 powder reaches about-32.9 dB at11.7 GHz,and its effective absorption bandwidth(RL -10 dB) is 2.6 GHz with the optimal matching thickness of 2.0 mm.     

Synthesis and characterization of CaAlxOy:Eu2+ phosphors prepared using solution-combustion method

Europium-doped calcium aluminate (CaAl_xO_y:Eu²⁺) phosphors were obtained at low temperatures (500 °C) by the solution - combustion of corresponding metal nitrate-urea solution mixtures. The particle size and morphology and the structural and luminescent properties of the as-synthesized phosphors were examined by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), Auger spectroscopy, transmission electron spectroscopy (TEM) and photoluminescence (PL). It was found that the Ca:Al molar ratios showed greatly influence not only on the particle size and morphology, but also on their PL spectra and structure. With the Ca: Al molar ratios increasing from 6:100 to 26:100, the structure of as-synthesized phosphor changed from CaAl₁₂O₁₉ to monoclinic CaAl₂O₄ and the dominant emitting light from red to blue, implying that the oxidation state of doped europium ions changed from trivalent to divalent due to the structure variation of host lattice. A blue phosphor with almost pure phase can be easily prepared by solution combustion method with suitable Ca:Al molar ratio.     

Preparation of high performance YGdBCO films by low fluorine TFA-MOD process

YBCO films doped with different contents of gadolinium(Gd) were prepared by the low-fluorine(low-F)trifluoroacetate metal-organic deposition(MOD) method.The effects of flow rate and holding time of the firing(crystallization) stage on the superconducting properties of Y_xGd_(1-x)Ba_2 Cu_3 O_(7-δ)(YGdBCO) films were investigated.The phase formation and texture were characterized by the X-ray diffraction(XRD),which indicate that severe degradation of the microstructure will be induced with the inappropriate flow rate.The surface morphology and element distribution were investigated by the scanning electron microscopy(SEM) and energy dispersive spectroscopy(EDS).The results show that increasing the holding time of the firing stage is effective for the further decomposition of residual impurity phase on the surface.The mechanisms of the phase and surface evolution are also discussed.Finally,a high critical current density(J_c) value of 5.4 MA/cm~2 was achieved in the Y_(0.9)Gd_(0.1)BCO film fabricated by the cooperative control of the flow rate and holding time of the firing stage,which are contributed to the formation of excellent texture,homogeneous microstructure and dense surface of the YGdBCO films.     

Influence of La-Co substitution on the structure and magnetic properties of low-temperature sintered M-type barium ferrites

La-Co substituted M-type barium ferrites (BaM) were prepared by traditional solid state method and sintered at low tem-perature (1173 K). X-ray diffraction (XRD), scanning electron microscopy (SEM) and...     

Phase relations,microstructure, and valence transition studies on CaZr_(1-x)Ce_xTi_2O_7(0.0≤x≤1.0) system

In this study, Ce-doped zirconolite was synthesized through high-temperature solid-state reaction at 1250 ℃ in air for 96 h. The crystal phase.microstructure and valence transition were studied by X-ray diffraction(XRD), scanning electron microscopy(SEM), and X-ray photoelectron spectroscopy(XPS).Phase relations of CaZr_(1-x)Ce_xTi_2O_7 systems were determined by XRD analyses and Rietveld refinements.Four different phases are identified, namely zirconolite, perovskite, pyrochlore, and cerianite. The phase transformation(2M-zirconolite → 4M-zirconolite → Ce-pyrochlore) is caused by cations rearrangement as cerium content increases. The solubility limit of cerium ions in CaZr_(1-x)Ce_xTi_2O_7 system is estimated to be approximately 0.80. Under sintering air atmosphere, partial reduction of Ce~(4+) in Ce~(3+) is detected in Ce 3d XPS spectra, and the ratio of Ce~(3+) and Ce~(4+) significantly decreases as cerium content increases.     

Magnetic properties and magnetization behavior of SmCo-based magnets with TbCu7-type structure

The nanocrystalline magnets with nominal compositions of Sm1-xLuxCo6.8Zr0.2(x=0,0.2,0.4,0.6)were prepared directly by the intensive milling.The effects of Lu content on the phase structure,the magnetic properties,and magnetization behaviors were also investigated.The XRD patterns of the as-milled samples showed a single SmCo7 phase with TbCu7 structure.Lu addition was proved to result in relevant improvements in the microstructure and magnetic properties,especially in the maximum energy product(BH)max.It was shown that a higher maximum energy product and coercivity of about 17.47 kJ/m3 and 473.45 kA/m were obtained in the sample with x=0.2.From the analysis of the magnetization reversal behavior,it was found that a stronger intergrain exchange coupling interaction was observed in the samples with Lu-doping.From the studies of the coercivity mechanism,it was shown that nucleation model was the dominant magnetization reversal process at the elevated temperature.     

Thermodynamic Basis of Non-equilibrium Phase Transformations of bcc β-Phase in Ti–Mo System

This study reports the experimental identification of transformation products of high temperature bcc β phase in Ti–xMo (x = 1, 7, 15, 25 wt%) alloys and aims to understand the transformations by thermodynamic modelling. The high temperature bcc β phase had undergone martensitic transformation in Ti–1Mo and Ti–7Mo alloys, resulting in acicular martensitic structure within large β grains. X-ray diffraction (XRD) analysis confirmed the martensite to be hcp (α′) and orthorhombic (α″) in Ti–1Mo and Ti–7Mo alloys respectively. Combined analysis of XRD and transmission electron microscopy (TEM) suggested the formation of fine plates of α″, omega (ω) and bcc β phases in Ti-15 and Ti-25 Mo alloys. Calculation of enthalpy of formation supported the stability of solid solution phase over the amorphous phase in the entire concentration range of Mo.     

Electrochemical hydrogen storage performances of the nanocrystalline and amorphous（Mg24 Ni10 Cu2）100-x Ndx（x=0–20） alloys applied to Ni-MH battery

Melt spinning technology was used to prepare the Mg2 Ni-type（Mg24 Ni10 Cu2）100–x Ndx（x=0,5,10,15,20） alloys in order to obtain a nanocrystalline and amorphous structure.The effects of Nd content and spinning rate on the structures and electrochemical hydrogen storage performances of the alloys were investigated.The structure characterizations of X-ray diffraction（XRD）,transmission electron microscopy（TEM） and scanning electron microscopy（SEM） linked with energy dispersive spectroscopy（EDS） revealed that the as-spun Nd-free alloy displayed an entire nanocrystalline structure,whereas the as-spun Nd-added alloys held a nanocrystalline and amorphous structure and the degree of amorphization visibly increased with the rising of Nd content and spinning rate,suggesting that the addition of Nd facilitated the glass forming of the Mg2 Ni-type alloy.The electrochemical measurements indicated that the addition of Nd and melt spinning improved the electrochemical hydrogen storage performances of the alloys significantly.The discharge capacities of the as-cast and spun alloys exhibited maximum values when Nd content was x=10,which were 86.4,200.5,266.3,402.5 and 452.8 mAh/g corresponding to the spinning rate of 0（As-cast was defined as the spinning rate of 0 m/s）,10,20,30 and 40 m/s,respectively.The cycle stability（S20,the capacity maintain rate at 20thcycle） of the as-cast alloy always rose with the increasing of Nd content,and those of the as-spun alloys exhibited the maximum values for Nd content x=10,which were 77.9%,83.4% 89.2% and 89.7%,corresponding to the spinning rate of 10,20,30 and 40 m/s,respectively.     

Crystal structure and magnetic properties of SmCo6.6Nb0.4 nanoflakes prepared by surfactant-assisted ball milling

SmCo6.6Nb0.4 nanoflakes with TbCu7 structure were successfully prepared by surfactant-assisted high energy ball milling （SA-HEBM） with heptane and oleic acid as milling medium. The microstructure, crystal structure and magnetic properties were stud- ied by scanning electron microscopy, X-ray diffraction, and vibrating sample magnetometer, respectively. The effects of ball milling time on the c-axis crystallographic alignment and coercivity of the nanoflakes were systematically investigated. The research showed that the nanoflakes had an average thickness of 100 nm, an average diameter of 1 μm, with an aspect ratio as high as 100. As the ball milling time increased from 2 to 8 h, the reflection peaks intensity ratio I（002y/I（10l）, which indicated the degree of c-axis crystal texture of the SmCo6.6Nbo.4 phase, increased first, reached a peak at 4 h, and then decreased. Meanwhile, the coercivity of the nanoflakes also increased first, reached a peak at 13.86 kOe for 4 h, and then decreased.     

P92钢中δ-铁素体内Laves相的长大规律

 用透射电镜、扫描电镜对两炉δ-铁素体含量不同的P92钢中的Laves相形貌与尺寸进行了分析与测量。结果表明：在时效状态下,δ-铁素体内也有Laves相析出,其尺寸显著大于马氏体基体中的Laves相;δ-铁素体含量越高,δ-铁素体内的Laves相尺寸与增长速度越大;δ-铁素体含量对马氏体基体中的Laves相尺寸影响不大。