Nondestructive evaluation of isothermally annealed 12% CrMoV steel by magnetic BN measurement

The effects of microstructural evolution during isothermal annealing on structure-sensitive magnetic properties and Barkhausen noise (BN) characteristics have been investigated for 12% CrMoV steel. A rapid decrease in coercive force, remanence, hysteresis loss and hardness took place in accordance with the release of internal stresses from supersaturated martensite after annealing for only 20 minutes at 923 K. BN energy is correspondingly related with three stages of microstructural evolution such as the recovery of strain energy, the increase of precipitates size as a result of Ostwald ripening and the annihilation of dislocation density during isothermal annealing of the specimen. The linear relation between hardness and BN parameters in the magnetization region of irreversible domain wall displacement of 2.4 kA/m suggests that hardness and microstructural evolution could well be evaluated nondestructively by using BN measurements.     

Accurate determination of the number density of G-phase precipitates in thermally aged duplex stainless steel

G-phase precipitation in the ferrite phase in thermally aged duplex stainless steel (DSS) was investigated. A needle-shaped sample of DSS aged at 673?K for 5000?h was observed by transmission electron microscopy (TEM), and subsequently by atom probe tomography (APT). The precipitates of the G-phase observed by TEM corresponded well to clustering atoms observed by APT. On the other hand, regarding the precipitates of the G-phase that formed in an earlier stage of aging, the present study suggests that not all the precipitates can be detected by TEM. A large area of DSS aged at 673?K for 5000?h containing both the ferrite and austenite phases was observed. The number density of precipitates of the G-phase in the ferrite phase was small in the vicinity of the phase boundary and increased with the distance between the phase boundary and each field of view. The number density reached an almost constant value at a distance of approximately 4?µm from the phase boundary. The suppression of G-phase precipitation in the vicinity of the phase boundary is discussed in terms of the depletion of alloying elements that comprise the G-phase.     

Microstructure and shape memory behaviour of annealed Ti51.5Ni(48.5- x )Cu x ( x = 6.5–20.9) thin films

Ti-rich Ti–Ni–Cu amorphous films (Ti_51.9Ni_41.6Cu_6.5, Ti_51.6Ni_36.8Cu_11.6, Ti_51.5Ni_33.1Cu_15.4 and Ti_51.7Ni_27.4Cu_20.9), formed by sputtering, were annealed at 773, 873 and 973?K for 1?h and their structures and shape memory behaviours investigated. All the films annealed at 773?K for 1?h exhibited Guinier–Preston (GP) zones, but these precipitates were absent after annealing at 873?K or higher. Instead of GP zones, coherent plate precipitates of a Ti₂Cu phase were formed in films annealed at 873?K for 1?h, when the Cu content was between 11.6 to 20.9 at.%. The strain–temperature curves under constant stresses of Ti_51.6Ni_36.8Cu_11.6 and Ti_51.5Ni_33.1Cu_15.4 films showed a two-step deformation associated with the B2???B19???B19′ transformation, whereas Ti_51.9Ni_41.6Cu_6.5 and Ti_51.7Ni_27.4Cu_20.9 films showed a single-step deformation associated with the B2?B19′ and B2?B19 transformations, respectively. The two kinds of plate precipitates, GP zones and a Ti₂Cu phase were found to be effective to increase the critical stress for plastic strain.     

Effects of aging temperature on G-phase precipitation and ferrite-phase decomposition in duplex stainless steel

G-phase precipitation and ferrite-phase decomposition in a cast duplex stainless steel (DSS) aged at 623–723?K for up to 8000?h were investigated using atom probe tomography (APT). Large sample volume was observed in every APT experiment, which yielded significantly statistical results. The number density of G-phase precipitates tended to be high and their sizes were small at lower aging temperatures. G-phase precipitates grew during prolonged isothermal aging. The concentrations of nickel, silicon, manganese and molybdenum in G-phase precipitates tended to increase as the precipitates grew. Heterogeneous distributions of alloying elements within G-phase precipitates were observed. An interesting positional relationship of G-phase precipitates with dislocations was revealed. Regarding the ferrite-phase decomposition, local chromium concentrations in the ferrite phase varied fast at higher aging temperatures. Good correlation between the variation of local chromium concentrations and aging conditions was revealed, which indicates that the variation can be estimated for arbitrary aging conditions. Representative distances between chromium-enriched and chromium-diluted regions were long at higher aging temperatures. Time exponent of the representative distances of ferrite-phase decomposition as well as the size of G-phase precipitates increased with aging temperatures.     

Isochronal annealing studies of deformed FeSi alloys using positron annihilation spectroscopy

A series of FeSi samples were deformed to a thickness reduction of 16%. They were isochronally annealed for one hour at different temperatures and characterized by the Doppler broadening of the annihilation radiation (DBAR) measured at room temperature. Optical microscopy (OM) is used to investigate the microstructure of the deformed samples before and after annealing. The S parameter data show a decrease with the increase of the annealing temperature. At 973 K a significant decrease sets in. The microstructures of the alloys, investigated by OM, show that recrystallization is completed at 1173 K.     

In situ SEM studies of the transformation sequence of multistage martensitic transformations in aged Ti-50.8 at.% Ni alloys

The transformation behaviour of the multistage martensitic transformation in aged Ti-50.8 at.% Ni alloys was investigated by differential scanning calorimetry (DSC) and in situ scanning electron microscopy (SEM). The specimens aged from 673 to 748?K for 3.6?ks under an unregulated heat treatment atmosphere exhibited the double-stage transformation during cooling. The quadruple-stage transformation was observed in the specimens aged at 773 and 798?K, and the triple-stage transformation appeared in the specimen aged at 823?K under an unregulated heat treatment atmosphere. The distribution and size of Ti₃Ni₄ precipitates were heterogeneous in these specimens. The single-stage transformation in the specimen aged at 848?K was similar to that of the solution-treated specimen. In the forward quadruple-stage transformation, the R-phase transformation occurred in the intermediate region and around the grain boundary. The first martensitic transformation, which corresponded to the M1 peak in the DSC cooling curve, took place in the intermediate region of grains via the R phase. The second transformation, which corresponded to the M2 peak, occurred around the grain boundary via the R phase. The final transformation, which corresponded to the M3 peak, arose directly from the B2 parent phase at the grain centre. The transformation sequence and areas described above were quantitatively verified by comparing the SEM observations with the DSC measurements. The transformation sequence of the triple-stage transformation was also discussed.     

Annealing dependence of magnetic properties in nanostructured Sm0.5Y0.5Co5

Nanocrystalline Sm_0.5Y_0.5Co₅ powders with high coercivity H_C and enhanced remanence M_r were prepared by mechanical milling and subsequent annealing. Annealing temperatures T ranging from 973 to 1173 K, and times t ranging from 1 to 5 min were used. X-ray diffraction (XRD) and DC-magnetization measurements were carried out to study the microstructure and magnetic properties of these samples. XRD patterns demonstrate that the average grain size D of the nanocrystalline powders depends on the annealing temperature T and time t: D ranges from 11 nm (for T=973 K and t=1 min) to 93 nm (for T=1173 K and t=5 min). Magnetic measurements performed at room temperature indicate high coercivity values (H_C>955 kA/m), and enhanced remanence (M_r/M_max>0.5) for all samples. A strong annealing-induced grain size dependence of these magnetic properties was found.     

Microstructural and optical properties of nanocrystalline undoped zirconia thin films prepared by pulsed laser deposition

The zirconium oxide (ZrO₂) thin films are deposited on Si (100) and quartz substrates at various substrate temperatures (room temperature–973 K) at an optimized oxygen partial pressure of 3×10^?2 mbar using pulsed laser deposition technique. The effect of substrate temperature on microstructural, optical and mechanical properties of the films is investigated. The X-ray diffraction studies show that the films deposited at temperatures ≤773 K are monoclinic, while the films deposited at temperatures ≥873 K show both monoclinic and tetragonal phases. Tetragonal phase content increases with the increase of substrate temperatures. The surface morphology and roughness are investigated using atomic force microscope in contact mode. The optical properties of the films show that the refractive indices (at 550 nm) are found to increase from 1.84 to 2.35 as the temperature raises from room temperature (RT) to 973 K. Nanoindentation measurements show that the hardness of the films is 11.8 and 13.7 GPa for the films deposited at 300 and 973 K, respectively.     

Effect of precipitates on thermal conductivity of aged Mg-5Sn alloy

Abstract

The influence of precipitates on thermal conductivity of aged Mg-5Sn alloy has been investigated at different heat treatment temperatures. The results show that the thermal conductivity of aged Mg-5Sn alloy increases from 87.5 to 92.8 W·m^?1·K^?1 at 433 K for 720 h and from 87.5 to 122 W·m^?1·K^?1 at 513 K for 120 h with the increasing ageing time. The increasing rate of the former is obviously lower than that of the latter. Meanwhile, the Sn content of precipitates at 433 K is considerably below that of aged Mg-5Sn at 513 K. The interface between precipitates and α-Mg matrix is completely coherent at 433 K for 720 h. The increase in thermal conductivity is mainly attributed to the remaining Sn solutes in α-Mg matrix, and the interface relationship between precipitates and α-Mg matrix.     

M?ssbauer study of the '11' iron-based superconductors parent compound Fe(1+x)Te

(57)Fe M?ssbauer spectroscopy was applied to investigate the superconductor parent compound Fe(1+x)Te for x?=?0.06, 0.10, 0.14, 0.18 within the temperature range 4.2-300?K. A spin density wave (SDW) within the iron atoms occupying regular tetrahedral sites was observed, with the square root of the mean square amplitude at 4.2?K varying between 9.7 and 15.7?T with increasing x. Three additional magnetic spectral components appeared due to the interstitial iron distributed over available sites between the Fe-Te layers. The excess iron showed hyperfine fields at approximately 16, 21 and 49?T for three respective components at 4.2?K. The component with a large field of 49?T indicated the presence of isolated iron atoms with large localized magnetic moments in interstitial positions. Magnetic ordering of the interstitial iron disappeared in accordance with the fallout of the SDW with increasing temperature.     

Ferromagnetic domain structures and nanoclusters in Nd(1/2)Sr(1/2)MnO3

Magnetic domain structures of Nd(1/2)Sr(1/2)MnO3 were investigated by means of low-temperature Lorentz electron microscopy. On cooling, magnetic domain walls started to appear at 250 K, and they were oriented straight along the [100] and [110] directions. With a further decrease in temperature, the volume of each magnetic domain increased with discontinuous domain-wall jumps. A characteristic granular image was observed at around 140 K, near the charge-ordering transition temperature. We consider that this originated from ferromagnetic nanoclusters that appeared in the antiferromagnetic matrix.     

Ferromagnetism in MnxGe1−x films prepared by magnetron sputtering

Mn_xGe_1−x thin films were prepared by magnetron sputtering with a substrate temperature of 673 K and subsequently annealed at 873 K. The X-ray diffraction (XRD) measurements showed that all samples had a single Ge cubic structure. No films showed clear magnetic domain structure under a magnetic force microscope (MFM). Atom force microscope (AFM) measurements showed that the films had an uniform particle size distribution, and a columnar growth pattern. X-ray photoelectron spectroscopy (XPS) measurements indicated that the valences of both Mn and Ge atoms increase with the Mn concentration. The resistance decreased with increasing temperature, suggesting that the films were typical semiconductors. Magnetic measurements carried out using a Physical Property Measurement System (PPMS) showed that all samples exhibited ferromagnetism at room temperature. There was a small concentration of Mn₁₁Ge₈ in the films, but the ferromagnetism was mainly induced by Mn substitution for Ge site.     

Abnormal magnetic behaviour of powder metallurgy austenitic stainless steels sintered in nitrogen

The magnetic response of AISI 304L and AISI 316L obtained through powder metallurgy and sintered in nitrogen were studied. AISI 304L sintered in nitrogen showed a ferromagnetic behaviour in as-sintered state while AISI 316L was paramagnetic. After solution annealing both were paramagnetic. Magnetic behaviour was analysed by using a vibrating sample magnetometer, a magnetic ferritscope and magnetic etching. A microstructural characterization was performed by means of optical metallography, X-ray diffraction, scanning electron microscopy (SEM) and energy dispersive analysis of X-rays (EDS). Some samples when needed were submitted to aged heat treatments at 675 and 875 °C for 90 min, 4, 6, 8 or 48 h. The main microstructural feature found was the presence of a lamellar constituent formed by nitride precipitates and an interlamellar matrix of austenite and/or ferrite. The abnormal magnetic response was explained based on this.     

Reentrant ferromagnetism observed in SmMn2Ge2

Magnetic characteristics of SmMn₂Ge₂ with a layer structure have been studied by magnetization measurements using single crystal. In the sequence of decreasing temperature, ferromagnetism is observed at 196 K ? T ? 348 K, collinear antiferromagnetism becomes stable for 64 K ? T < 196 K and reentrant ferromagnetism appears below 64 K. The appearance of such successive magnetic orderings are attributed to the variation of the shortest Mn-Mn distance due to thermal expansion and the existence of ferromagnetic coupling between the Sm moments in the intralayer which is dominant at low temperatures.     

Magnetic correlations at graphene edges: basis for novel spintronics devices

Magnetic zigzag edges of graphene are considered as a basis for novel spintronics devices despite the fact that no true long-range magnetic order is possible in one dimension. We study the transverse and longitudinal fluctuations of magnetic moments at zigzag edges of graphene from first principles. We find a high value for the spin wave stiffness D=2100 meV A2 and a spin-collinear domain wall creation energy E(dw)=114 meV accompanied by low magnetic anisotropy. Above the crossover temperature T(x) approximately 10 K, the spin correlation length xi proportional, variantT(-1) limits the long-range magnetic order to approximately 1 nm at 300 K while below T(x), it grows exponentially with decreasing temperature. We discuss possible ways of increasing the range of magnetic order and effects of edge roughness on it.     

Magnetic studies on ZnTe:Cr film grown on glass substrate by thermal evaporation method

ZnTe and ZnTe:Cr films were prepared on glass substrate by using thermal evaporation method. X-ray diffraction analysis revealed the presence of ZnCrTe phase. X-ray photoelectron spectroscopy was used to estimate the composition of as-prepared films. The valence state of Cr in ZnTe:Cr film is determined to be +2 by using electron spin resonance spectroscopy. Magnetic moment data as a function of magnetic field was recorded by using superconducting quantum interference device magnetometry at 300 K. The result showed a clear hysteresis loop with coercive field of 48 Oe. Magnetic domains were observed by using magnetic force microscopy and the average value of domain size was 3.7 nm.     

Microstructures and magnetic properties of Fe---Pt permanent magnets

We have investigated the magnetic properties of Fe---38.5Pt, Fe---39.5Pt and Fe---50.0Pt (at%) alloys after various heat treatment conditions using a vibrating sample magnetometer, and correlated these properties with the microstructures of the alloys by transmission electron microscopy. The Fe---50Pt alloy shows poor magnetic hardness regardless of the heat treatment conditions. The magnetic hardness of the Fe---39.5Pt alloy shows a maximum value after annealing for 10 h at 873 K, while it monotonically decreases after annealing at 1073 K. The alloy with the highest coercivity was composed of a single phase γ₁ with an average domain size of approximately 10 nm. The electron diffraction results indicate that the alloy is frustrated with accumulated stress, induced by a cubic → tetragonal transformation which occurs without twinning. On the other hand, when stress is relieved by twin formation after prolonged aging, the coercivity decreases. By annealing at 1073 K, the well known polytwin structure evolves. However, only poor hard magnetic properties are observed when this polytwin structure appears. Hence, the highest coercivity is attributed to the formation of nanoscale L1₀ ordered antiphase domains which is expected to be a highly anisotropic single domain magnetic particle.     

Microstructure of annealed Ti48.5Ni(51.5– x )Cu x (x = 6.2–33.5) thin films

(Ni, Cu)-rich Ti–Ni–Cu amorphous films with a Cu content of 6.2–33.5 at. % formed by sputtering were annealed at 773, 873 and 973 K for 1 h and their microstructures investigated. Two types of precipitate were observed in the annealed films: a Ti(NiCu)₂ phase for the Ti_48.5Ni₄₀Cu_11.5, Ti_48.6Ni_35.9Cu_15.5, Ti_48.3Ni_28.4Cu_23.3 and Ti_48.3Ni_23.9Cu_27.8 films, plus a TiCu phase for the Ti_48.5Ni₁₈Cu_33.5 films. These precipitates were found to have coherency with the B2 matrix in the films annealed at 773 K and were densely distributed within the grains. However, in the films annealed at 873 K, their size increased 10-fold and their density decreased. Annealing at 973 K promoted grain-boundary precipitation and, accordingly, the density of the precipitates in the grain interiors decreased. On the other hand, the annealed Ti_48.9Ni_44.9Cu_6.2 films showed no precipitates in their grain interiors, but the number of grain-boundary precipitates increased with increasing annealing temperature. It was also found that grain size decreased with increasing Cu content and was significantly decreased for the Ti_48.5Ni₁₈Cu_33.5 films.     

Magnetoelectric memory effect in the Y-type hexaferrite BaSrZnMgFe_(12)O_(22)

We report on the magnetic and magnetoelectric properties of the Y-type hexaferrite BaSrZnMgFe_(12)O_(22),which undergoes transitions from a collinear ferrimagnetic phase to a proper screw phase at 310 K and to a longitudinal conical phase at 45 K.Magnetic and electric measurements revealed that the magnetic structure with spiral spin order can be modified by applying a magnetic field,resulting in magnetically controllable electric polarization.It was observed that BaSrZnMgFe_(12)O_(22)exhibits an anomalous magnetoelectric memory effect:the ferroelectric state can be partially recovered from the paraelectric phase with collinear spin structure by reducing magnetic field at 20 K.We ascribe this memory effect to the pinning of multiferroic domain walls,where spin chirality and structure are preserved even in the nonpolar collinear spin state.     

Synthesis of nickel nanoparticles in silica by alcogel electrolysis

We report a novel technique for the formation of metal nanoparticles, based on electrolysis of the alcogels containing metal chlorides. The alcogel was formed from TEOS, water, ethanol, and nickel chloride, and subjected to galvanostatic electrolysis. This resulted in successful formation of Ni nanoparticles inside the silica gel. Average particle size of FCC Ni lies between 18 and 20 nm. The formation of tetragonal nickel (a sub-oxide of nickel) as well as NiO were also detected by XRD and SAED. The resistivity measurements showed that the nickel nanoparticles were separated from each other by Ni(O) present between them. Magnetic studies based on ZFC and FC measurements below room temperature (up to 5 K) and above room temperature (up to 700 K) were conducted using SQUID and Magnetic TGA, respectively, which showed strong magnetic irreversibility as attributable to exchange interaction between metallic and oxide phases and mutual interactions among metallic particles in the network structure. The blocking temperature (~600 K) of the samples was above room temperature. M–H studies based on VSM showed an increase in magnetic coercivity with the formation of NiO. A magnetic transition associated with tetragonal nickel was seen at 10 K.