Effect of annealing prior to cold rolling on magnetic and mechanical properties of low carbon non-oriented electrical steels

The effects of annealing prior to cold rolling on the microstructure, magnetic and mechanical properties of low-C grain non-oriented (GNO) electrical steels have been investigated. The grain structure of hot-rolled electrical steel strips is modified by annealing at temperatures between 700 and 1050 °C. Annealing at temperatures less than the ferrite to austenite+ferrite transformation temperature on heating (Ac₁) causes a marginal effect on the grain size. However, annealing in the intercritical region at temperatures between Ac₁ and Ac₃ (the ferrite+austenite to austenite transformation temperature on heating) causes rapid decarburization and development of large columnar ferrite grains free of carbide particles. This microstructure leads, after cold rolling and a fast annealing treatment, to carbide free, large ferrite grain microstructures with magnetic and mechanical properties superior to those observed typically in the same steel in the industrially fully processed condition. These results are attributed to the increment in grain size and to the {1 0 0} fiber texture developed during the final annealing at temperatures up to 850 °C. Annealing at higher temperatures, T>Ac₃, results in a strong {1 1 1} fiber texture and an increase of the quantity of second phase particles present in the microstructure, which lead to a negative effect on the final properties. The results suggest that annealing prior to cold rolling offers an attractive alternative processing route for the manufacture of fully processed low C GNO electrical steels strips.     

Investigation of microstructural changes in M250 grade maraging steel using positron annihilation

Microstructural evolution of M250 grade maraging steel subjected to various thermal-aging treatments has been investigated using positron annihilation, X-ray diffraction, hardness and electron microscopy studies. Isochronal aging treatment in the range of 600–900 K, in steps of 100 K, was carried out and positron lifetime, austenite volume fraction and hardness values have been measured. The stages corresponding to point defect dynamics and formation of intermetallics have been clearly identified. Based on these results, measurements were performed on specimens isothermally aged at 755 K from 0.1 to 100 h to elucidate the time evolution of microstructural changes, and the results are discussed.     

Magnetic and optical properties of self-organized InMnAs quantum dots

Ten layers of self-assembled InMnAs quantum dots with InGaAs barrier were grown on high resistivity (1 0 0) p-type GaAs substrates by molecular beam epitaxy (MBE). The presence of ferromagnetic structure was confirmed in the InMnAs diluted magnetic quantum dots. The ten layers of self-assembled InMnAs quantum dots were found to be semiconducting, and have ferromagnetic ordering with a Curie temperature, T_C=80 K. It is likely that the ferromagnetic exchange coupling of sample with T_C=80 K is hole mediated resulting in Mn substituting In and is due to the bound magnetic polarons co-existing in the system. PL emission spectra of InMnAs samples grown at temperature of 275, 260 and 240 °C show that the interband transition peak centered at 1.31 eV coming from the InMnAs quantum dot blueshifts because of the strong confinement effects with increasing growth temperature.     

Surface and subsurface stress evaluation in case-carburised steel using high and low frequency magnetic barkhausen emission measurements

The effect of near-surface and subsurface stresses on the magnetic Barkhausen emission (MBE) profile has been studied in case-carburised and tempered En36 steel. The high- and low-frequency MBE measurements were made, on both tensile and compressive sides of the rectangular bar specimens with case-depth of 0.95 mm loaded in cantilever beam, under different stress levels as well as after unloading from different higher stress levels. The high-frequency MBE profile showed a single peak while the low-frequency MBE profile showed two peaks. Under applied elastic stresses, both types of measurement showed increase in MBE under tension and decrease in MBE under compression. But, the MBE profiles measured after unloading from higher stresses showed different behaviour. On the tensile side, the high-frequency MBE profile did not change significantly due to pre-stress. But, in the low-frequency MBE profile, the first peak increases and the second peak decreases with increase in pre-stress. On the compressive side, the peak height of high-frequency MBE profile decreased gradually with increase in pre-stress. The first peak of the low-frequency MBE profile also decreased gradually with increase in pres-stress level. But, the second peak of the low-frequency MBE profile decreased by about 10% at a pre-stress level of −1094 MPa and remained more or less the same even after unloading from −1783 MPa. The MBE behaviour has been correlated to the residual stress (RS)-depth profile measured using X-ray diffraction method. This correlation clearly indicates that the high-frequency MBE reflects only the changes in surface RS level. It does not indicate RS changes occurring at depths >20 μm below the surface. The low-frequency MBE profile reflects the changes in the RS distribution occurring in the near-surface as well as deeper subsurface layers.     

Preparation of non-oriented silicon steel with high magnetic induction using columnar grains

Columnar grains can lead to detrimental surface ridging and an inhomogeneous microstructure, although their {1 0 0}〈0 v w〉 texture is considered desirable due to their good magnetic properties in non-oriented silicon steel. Based on the hereditary tendency of {1 0 0}〈0 v w〉 texture, the effects of lubrication and heating rate on texture and on final magnetic properties were investigated using a cast slab containing 100% columnar grains. Hot rolling with lubrication, normalization at low heating rate, two-stage cold rolling, and final annealing at 1000 °C helped achieve high performance. As a result, a new non-oriented silicon steel with high magnetic induction (B₅₀=1.82 T) and low core loss (P_1.5=2.35 W/kg) was prepared. The possibility of further performance optimization was also discussed.     

Structure, magneto-structural transitions and magnetocaloric properties in Ni50−xMn37+xIn13 melt spun ribbons

Melt spun Ni_50−xMn_37+xIn₁₃ (2≤x≤5) ribbons were investigated for the structure, microstructure, magneto-structural transitions and inverse magnetocaloric effect (IMCE) associated with the first-order martensitic phase transition. The influence of excess Mn in Ni site (or Ni/Mn content) on the martensite transition and the associated magnetic and magnetocaloric properties are discussed. It was found that with the increase in Mn content, the martensitic transition shifted from 325 to 240 K as x is varied from 2 to 4, and the austenite phase was stabilized at room temperature. The x=5 ribbon did not show the martensitic transition. For the x=3 ribbon, the structural and magnetic transitions are close together unlike in the x=4 ribbon in which they are far (∼60 K) apart. The zero field cooled and field cooled curves support the presence of exchange bias blocking temperature due to antiferromagnetic interactions in the ribbons. A large change in the magnetization between the martensite and austenite phases was observed for a small variation in the Ni/Mn content, which resulted in large IMCE. A large positive magnetic entropy change (ΔS_M) of 32 J/kg K at room temperature (∼ 300 K) for a field change of 5 T with a net refrigeration capacity of 64 J/kg was obtained in the Ni₄₇Mn₄₀In₁₃ ribbon.     

Influence of chemistry and hot rolling conditions on high permeability non-grain oriented silicon steel

This paper discusses the influence of chemical composition on the final electromagnetic properties in higher permeability material. Furthermore, the effect of the hot rolling practice and the end of austenite transformation temperature range on the hot band microstructure is described. The magnetic polarization J₅₀₀₀ better than 1.7 T, using hot rolling conditions 40 mm transfer bar thickness, finish mill entry temperature 1000 °C, and finishing temperature 800–840 °C and after decarburization heat treatment and grain growth treatment, was obtained.     

Effect of sputtering power on surface topography of dc magnetron sputtered Ti thin films observed by AFM

Titanium films were deposited on glass substrates at room temperature by direct current (dc) magnetron sputtering at fixed Ar pressure of 1.7 Pa and sputtering time of 4 min with different sputtering power ranging from 100 to 300 W. Atomic force microscopy (AFM) was used to study topographic characteristics of the films, including crystalline feature, grain size, clustering and roughening. The amorphous-like microstructure feature has been observed at 100-150 W and the transition of crystal microstructure from amorphous-like to crystalline state occurs at 200 W. The increase in grain size of Ti films with the sputtering power (from 200 to 300 W) has been confirmed by AFM characterization. In addition, higher sputtering power (300 W) leads to the transformation of crystal texture from globular-like to hexagonal type. The study has shown that higher sputtering power results in the non-linear increase in deposition rate of Ti films. Good correlativity between the surface roughness parameters including root mean square (RMS) roughness, surface mean height (Ra) and maximum peak to valley height (P-V) for evaluating the lateral feature of the films has been manifested. Surface roughness has an increasing trend at 100-250 W, and then drops up to 300 W.     

Electric and magnetic signatures of martensitic and intermartensitic transformations in Ni-Mn-Ga crystal

Results are reported on the temperature dependence of resistivity (200≤T≤360 K) and low-field magnetization (5≤T≤350 K) for the off-stoichiometric Ni₄₉Mn₂₉Ga₂₂ single crystal. Measurements are made for both heating and cooling cycles. The resistivity data show two first-order (hysteretic) transformations centered at about 340 and 250 K. The magnetization data show the same two transformations as the resistivity data as well as a third centered at 285 K. The results are consistent with a martensite/austenite transformation near 340 K and two intermartensitic transformations centered at 285 and 250 K (three martensite phases).     

Optical characterization of InxGa1−xN alloys

InGaN layers were grown by molecular beam epitaxy (MBE) either directly on (0 0 0 1) sapphire substrates or on GaN-template layers deposited by metal-organic vapor-phase epitaxy (MOVPE). We combined spectroscopic ellipsometry (SE), Raman spectroscopy (RS), photoluminescence (PL) and atomic force microscopy (AFM) measurements to investigate optical properties, microstructure, vibrational and mechanical properties of the InGaN/GaN/sapphire layers.The analysis of SE data was done using a parametric dielectric function model, established by in situ and ex situ measurements. A dielectric function database, optical band gap, the microstructure and the alloy composition of the layers were derived. The variation of the InGaN band gap with the In content (x) in the 0 < x ≤ 0.14 range was found to follow the linear law E_g = 3.44-4.5x.The purity and the stability of the GaN and InGaN crystalline phase were investigated by RS.     

Influence of the nitrogen contents on the permeability characteristics and soft magnetic properties of FeHfN films

High permeability magnetic films can enhance the inductance of thin-film inductors in DC-DC converters. In order to obtain high permeability, the uniaxial anisotropy and coercivity should be as low as possible. This study employed dc reactive magnetron sputtering to fabricate nanocrystalline FeHfN thin films. The influence of the nitrogen flow on the composition, microstructure, and permeability characteristics, as well as magnetic properties was investigated. Increasing the nitrogen content can alter FeHfN films from amorphous-like to crystalline phases. The magnetic properties and permeability depend on variations in the microstructure. With the optimum N₂/Ar flow ratio of 4.8% (N₂ flow: 1.2 sccm), low anisotropy (H_K = 18 Oe), low coercivity (H_C = 1.1 Oe) and high permeability (μ′ > 600 at 50 MHz) were obtained for fabrication of a nanocrystalline FeHfN film with a thickness of around 700 nm. Such as-fabricated FeHfN films with a permeability of over 600 should be a promising candidate for high-permeability ferromagnetic material applications.     

Evolution of magnetic phase at low aging temperature in a heavily cold-drawn stainless steel fiber

The evolution of the magnetic phase upon aging at 300–520 °C in a heavily cold-drawn AISI 316L austenitic stainless steel fiber was studied using thermomagnetic analysis (TMA) and magnetic force microscopy with a heating stage. An increasing trend of magnetization from 50 °C to around 470 °C in the heating curves of TMA in austenitic stainless steels after a cold-drawing process was observed. No significant M_s temperature signal in the TMA curve at cooling indicated an increase in magnetization upon cooling period without significant phase transformation. A series of in situ magnetic force microscopy observations reveal a growth of the magnetic domain structure after aging at 300 °C for 2.5 h. Results show that the ferromagnetic increase during aging at lower annealing temperature resulted from the growth of martensite.     

Sequence of structural and magnetic transitions in Ni48Co2Mn39Sn11 shape memory alloy

The structural and magnetic transitions in Ni₄₈Co₂Mn₃₉Sn₁₁ shape memory alloy were systematically investigated. During cooling, the paramagnetic austenite transforms into paramagnetic martensite at T_M∼375 K, followed by a gradual transition from paramagnetic to superparamagnetic martensite around T_S∼320 K. Upon further cooling through T_P∼100 K, the superparamagnetic clusters collectively freeze into a superspin glass state as corroborated by aging, rejuvenation, and memory effects. Consequently, the unique transition sequence of paramagnetic austenite→paramagnetic martensite→superparamagnetic martensite→superspin-glass martensite is disclosed.     

Effect of oxygen pressure on microstructure and magnetic properties of strontium hexaferrite (SrFe12O19) film prepared by pulsed laser deposition

The effects of oxygen pressure during deposition on microstructure and magnetic properties of strontium hexaferrite (SrFe₁₂O₁₉) films grown on Si (100) substrate with Pt (111) underlayer by pulsed laser deposition have been investigated. X-ray diffraction pattern confirms that the films have c-axis perpendicular orientation. The c-axis dispersion (Δθ₅₀) increases and c-axis lattice parameter decreases with increasing oxygen pressure. The films have hexagonal shape grains with diameter of 150-250 nm as determined by atomic force microscopy. The coercivities in perpendicular direction are higher than those in in-plane direction, which shows the films have perpendicular magnetic anisotropy. The saturation magnetization and anisotropy field for the film deposited in oxygen pressure of 0.13 mbar are comparable to those of the bulk strontium hexaferrite. Higher oxygen pressure leads to the films having higher coercivity and squareness. The coercivity in perpendicular and in-plane directions of the film deposited in oxygen pressure of 0.13 mbar are 2520 Oe and 870 Oe, respectively.     

Effects of V2O5 addition on NiZn ferrite synthesized using two-step sintering process

The combined influence of a two-step sintering (TSS) process and addition of V₂O₅ on the microstructure and magnetic properties of NiZn ferrite was investigated. As comparison, samples prepared by the conventional single-step sintering (SSS) procedure were also studied. It was found that with 0.3 wt% V₂O₅ additive, the sample sintered by the two-step sintering process at a high temperature of 1250 °C for 30 min and a lower temperature of 1180 °C for 3 h exhibited more homogeneous microstructure and higher permeability with a high Q-factor. The results showed that the TSS method with suitable additive brought positive improvement of the microstructure and magnetic properties of NiZn ferrite.     

Study of high-temperature ageing and creep on bainitic 5Cr-0.5Mo steel by magnetic NDE techniques

5Cr-0.5Mo steel having initial bainitic microstructure has been aged at 600 °C for 5000 h and subjected to creep at 600 °C/60 MPa. At different lengths of time the tests were interrupted for magnetic measurement using magnetic Barkhausen emissions (MBE) and magnetic hysteresis loop (MHL) techniques. Composition, morphology and distribution of carbides were studied using scanning electron microscopy (SEM). Magnetic softness was observed in the material up to 1600 h of ageing due to the decrease in pinning density for the coarsening of carbides by accumulation of large number of finer carbides. At higher ageing periods the demagnetizing field offered by the large massive carbides causes magnetic hardening. During creep test since the material has been normalized at 50 h of creep test also the structural change in creep test is accelerated, the magnetic softening for the interstitial carbon migration to the grain boundary and stress relaxation has removed in such early periods of ageing. When the carbides started coarsening the number density of the carbides decreased and inter-carbide distance increased which enhances the magnetic softening in the material in the secondary stage of creep. Formation of massive carbides and micro voids at the late tertiary stage of creep offers demagnetizing field causes magnetic hardening before failure of the material.     

马氏体时效钢的时效结构

本文利用透射电子显微相和电子衍射相对18Ni马氏体时效钢中沉淀强化相和时效结构的结晶学性质进行了研究。利用数个不同晶带的衍射相,一致地鉴别出同时存在Ni₃Mo,Ni₃Ti沉淀相和弥散的逆转变奥氏体,并且确定了它们相对马氏体基体的取向关系。证明了沉淀相、逆转变奥氏体与基体之间,密排面和密排方向都相互平行。指出在透射电子显微相中看到的魏氏型沉淀结构,实际上是由棒状沉淀相构成的三维空间格条结构,其中棒状沉淀相的长度方向平行于基体的四个〈111〉型方向。所观察到的扩张位错和位错塞积的真实性需要更多的实验证实。从结构观点,讨论了沿位错线的沉淀过程,并提出了钴钼交互作用的可能机制。     

Optimization of VI/II pressure ratio in ZnTe growth on GaAs(0 0 1) by molecular beam epitaxy

ZnTe epilayers were grown on GaAs(0 0 1) substrates by molecular beam epitaxy (MBE) at different VI/II beam equivalent pressure (BEP) ratios (R_VI/II) in a wide range of 0.96-11 with constant Zn flux. Based on in situ reflection high-energy electron diffraction (RHEED) observation, two-dimensional (2D) growth mode can be formed by increasing the R_VI/II to 2.8. The Te/Zn pressure ratios lower than 4.0 correspond to Zn-rich growth state, while the ratios over 6.4 correspond to Te-rich one. The Zn sticking coefficient at various VI/II ratios are derived by the growth rate measurement. The ZnTe epilayer grown at a R_VI/II of 6.4 displays the narrowest full-width at half-maximum (FWHM) of double-crystal X-ray rocking curve (DCXRC) for (0 0 4) reflection. Atomic force microscopy (AFM) characterization shows that the grain size enlarges drastically with the R_VI/II. The surface root-mean-square (RMS) roughness decreases firstly, attains a minimum of 1.14 nm at a R_VI/II of 4.0 and then increases at higher ratios. It is suggested that the most suitable R_VI/II be controlled between 4.0 and 6.4 in order to grow high-quality ZnTe epitaxial thin films.     

Native oxidation of ultra high purity Cu bulk and thin films

The effect of microstructure and purity on the native oxidation of Cu was studied by using angle-resolved X-ray photoelectron spectroscopy (AR-XPS) and spectroscopic ellipsometry (SE). A high quality copper film prepared by ion beam deposition under a substrate bias voltage of −50 V (IBD Cu film at V_s = −50 V) showed an oxidation resistance as high as an ultra high purity copper (UHP Cu) bulk, whereas a Cu film deposited without substrate bias voltage (IBD Cu film at V_s = 0 V) showed lower oxidation resistance. The growth of Cu₂O layer on the UHP Cu bulk and both types of the films obeyed in principle a logarithmic rate law. However, the growth of oxide layer on the IBD Cu films at V_s = 0 and −50 V deviated upward from the logarithmic rate law after the exposure time of 320 and 800 h, respectively. The deviation from the logarithmic law is due to the formation of CuO on the Cu₂O layer after a critical time.     

The transport and magnetic properties of La–Pb–Mg–Mn–O manganites at low temperatures

The structure, transport properties and the magnetoresistance behavior in the temperature interval 77–400 K of the perovskite-like lanthanum manganites La_0.6Pb_0.4−xMg_x+yMnO₃ (x=0, 0.1, 0.2 and y=0, 0.2) were investigated. Polycrystalline bulk samples were prepared by sol–gel self-combustion and subsequent heat treatment at 1000 °C for different times, 40, 80, 160 and 320 min. All manganites exhibit a peak in the resistivity around 200–250 K, below the ferromagnetic ordering temperature (320–330 K). An isotropic and negative magnetoresistance has been observed in all compounds. Magnetoresistance MR exhibits a peak in the temperature range 130–150 K, below SC–metal transition temperature. Magnitude of MR at the peaks was nearly 27% in the magnetic field of 2 T. At room temperature, a magnetoresistance of 9.5% for La_0.6Pb_0.2Mg_0.2MnO₃ composition was obtained. Longer heat treatment time enhanced the magnetorezistive properties.