Treatment of misorientation data to determine the fraction of recrystallized grains in a partially recrystallized metal

A method has been developed to differentiate recrystallized from unrecrystallized grains in partially annealed samples based on the point-to-point misorientation within the grains. Recrystallized grains exhibit a low average point-to-point misorientation whereas the contrary is the case for deformed grains. The analysis for recrystallized fraction was calibrated based on this distinguishing feature, and it was found that the average point-to-point misorientation within a grain in a fully recrystallized sample was less than 0.7°. Based on this calibration, partially recrystallized samples were analysed for their degree of recrystallization, and the technique was validated using microhardness measurements. The analysis of the misorientation data was in excellent agreement with the hardness data. There are three factors which distinguish the current method in comparison to the earlier work: a fixed limit is maintained on the minimum number of pixels which may constitute a grain; pattern quality is not considered; and the recrystallization criterion is calibrated to the experimental data. Nevertheless, in the early stages of annealing, where recovery is likely to have the most influence on the drop in hardness, the analysis of electron backscattered diffraction (EBSD) data underpredicts the recrystallized fraction. The analysis was also conducted on a cold-rolled, nonannealed sample, and from this, the error of the technique is estimated to be a maximum of 0.06 recrystallized volume fraction.     

Effect of Mg Addition on the Ferrite Grain Boundaries Misorientation in HAZ of Low Carbon Steels

The relation between the Mg treatment and ferrite grain boundaries misorientation was investigated.The orientation imaging microscopy technique based on electron backscattered diffraction technique(EBSD) was used in this work.It was found that the addition of 0.005 wt% Mg to the steel could evidently increase the ratio of acicular ferrite crystals appearing at large angles boundaries to each other,which was attributed to the nucleation of the second-phase particles by the Mg treatment.The EBSD techniques provide a powerful method to characterize and quantify the ferrite grain boundaries misorientation,in order to relate it to toughness.     

Analysis of Orange Peel Defect in St14 Steel Sheet by Electron Backscattered Diffraction (EBSD)

In this paper, the orange peel defect in the surface range of the st14 steel sheet has been investigated using the electron backscattered diffraction (EBSD) technique. It has been found that the orange peel defect in the st14steel sheet was resulted from the local coarse grains which were produced during hot-rolling due to the critical deformation in dual-phase zone. During deep drawing, the coarse grains with {100}＜001＞ microtexture can slip on the {112}＜111＞ slip system to form bulging and yields orange peel defects, while the coarse grains with {112}＜110＞orientation do not form the defect as the Schmid factor of {112}＜111＞ slip system in it equals zero.     

Low temperature annealing effects on the structure and optical properties of ZnO films grown by pulsed laser deposition

ZnO thin films were deposited on glass substrates at room temperature (RT) ∼500 °C by pulsed laser deposition (PLD) technique and then were annealed at 150-450 °C in air. The effects of annealing temperature on the microstructure and optical properties of the thin films deposited at each substrate temperature were investigated by XRD, SEM, transmittance spectra, and photoluminescence (PL). The results showed that the c-axis orientation of ZnO thin films was not destroyed by annealing treatments; the grain size increased and stress relaxed for the films deposited at 200-500 °C, and thin films densified for the films deposited at RT with increasing annealing temperature. The transmittance spectra indicated that E_g of thin films showed a decreased trend with annealing temperature. From the PL measurements, there was a general trend, that is UV emission enhanced with lower annealing temperature and disappeared at higher annealing temperature for the films deposited at 200-500 °C; no UV emission was observed for the films deposited at RT regardless of annealing treatment. Improvement of grain size and stoichiometric ratio with annealing temperature can be attributed to the enhancement of UV emission, but the adsorbed oxygen species on the surface and grain boundary of films are thought to contribute the annihilation of UV emission. It seems that annealing at lower temperature in air is an effective method to improve the UV emission for thin films deposited on glass substrate at substrate temperature above RT.     

Effect of Compression with Oscillatory Torsion Processing on Structure and Properties of Cu

The results presented in this study were concerned with microstructures and mechanical properties of polycrystalline Cu subjected to plastic deformation by a compression with oscillatory torsion process. Different deformation parameters of the compression with oscillatory torsion process were adopted to study their effects on the microstructure and mechanical properties. The deformed microstructure was characterized quantita- tively by electron backscattered diffraction (EBSD) and scanning transmission electron microscopy (STEM). Mechanical properties were determined on an MTS QTest/10 machine equipped with digital image correlation. From the experimental results, processes performed at high compression speed and high torsion frequency are recommended for refining the grain size. The size of structure elements, such as average grain size (D) and subgrain size (d), reached 0.42 μm and 0.30 μm, respectively, and the fraction of high angle boundaries was 35% when the sample was deformed at a torsion frequency f = 1.6 Hz and compression rate v = 0.04 mm/s. These deformation parameters led to an improvement in the strength properties. The material exhibited an ultimate tensile strength (UTS) of 434 MPa and a yield strength (YS) of 418 MPa. These values were about two times greater than those of the initial state.     

Influences of Thermal Martensites and Grain Orientations on Strain-induced Martensites in High Manganese TRIP/TWIP Steels

Strain-induced martensites in high manganese TRIP/TWIP steels were investigated in the presence of thermal martensites and under the influence of austenitic grain orientation by X-ray diffraction(XRD),scanning electron microscopy(SEM) and electron backscattered diffraction(EBSD).Before deformation,the morphology of α’-M depended mainly on the number of variants and growing period.Regardless of martensite morphologies and deformation,the Kurdjumov-Sachs(K-S) orientation relationships always maintained.The 6 α-M variants formed from a plate of ε-M were of 3 pairs of twins with a common axis <110> α’ parallel to the normal of {111} γ habit plane to minimize transformation strain.When α’-M could be formed only by deformation,it nucleated at the intersection of ε-M variants and grew mainly in thick ε-M plates.Thick ε plates promoted significantly the α’-M and weakened the influence of grain orientations.During tension,the transformation in <100>-oriented grains was observed to be slower than that in <111>-oriented grains.Deformation twins promoted ε-M formation slightly and had no apparent effect on α’-M.Deformation increased the number of ε-M variants,but reduced that of α’-M variants.     

Uniform texture in Al-Zn-Mg alloys using a coupled force field of electron wind and external load

Cylindrical Al-Zn-Mg alloys were processed by electroplastic compression with forced air cooling.Compared to a simple compression process,an unequal intensity of {110} <111> was obtained,and other textures were eliminated by electroplastic compression,that is,electroplastic compression can promote a uniform texture.The various textures formed in different regions along the radial direction under a simple compression process were illuminated by analyzing the relationship between the crystal rotation and stress state.Furthermore,the interaction between the electrons and dislocations was studied in electroplastic compression.The electrons enhanced {110} <111> by promoting slipping of the dislocations when the Burgers vectors of the dislocations were parallel to the drift direction of the electrons.However,the electrons also inhibited crystal rotation by pinning the dislocations with the Burgers vectors perpendicular to the drift direction of the electrons.Therefore,textures other than {110} <111>have difficulty forming under electroplastic compression.The effect of the current energy on the texture(enhancement or attenuation) was in accordance with the law of conservation.The results provided reasonable explanations for the test phenomena.     

Investigation of Dislocation Microstructures Formed in Heavily Deformed Metals Through the Combined Use of EBSD and TEM

New applications of the electron back scattering diffraction (EBSD) technique for studying dislocation microstructures are presented. Examples from copper and steel samples are given to illustrate the links between crystallographic measurements and dislocation microstructure. The purpose of combining transmission electron microscopy (TEM) and EBSD is to obtain quantitative information about the evolution and heterogeneity of the dislocation microstructure, and how it depends on the texture of the material.     

正火温度对Nb-V-Ti微合金化大截面锻材Q345E钢组织与韧性的影响

采用热膨胀法测定了Nb-V-Ti微合金化Q345E钢的相变临界温度Ac1和Ac3,使用45kW箱式电阻炉对实验钢进行了正火处理,利用光学显微镜(OM)、扫描电镜(SEM)、电子背散射衍射(EBSD)和透射电镜(TEM)观察了正火后试样的组织演变规律,分析了正火温度对组织与低温韧性的影响。结果表明,Q345E钢的Ac1约732℃、Ac3约871℃;当正火温度为820℃和850℃时,组织由针状珠光体和未发生重结晶的粗大原始铁素体构成,针状珠光体由针状奥氏体转变而来,相邻针状珠光体中的铁素体相具有相同的晶体取向特征;当正火温度不低于880℃时,组织由重结晶后的铁素体和珠光体构成,随正火温度的提高组织尺寸逐渐增大;当正火温度为820~940℃时,随正火温度的提高冲击功呈现先增加后降低的变化规律,组织类型、尺寸、形态和均匀性是影响大截面锻材Q345E低温韧性的主要因素。     

Effect of annealing temperature on the tribological behavior of ZnO films prepared by sol-gel method

The tribological behavior of zinc oxide (ZnO) films grown on glass and silicon (100) substrates by sol-gel method was investigated. Particularly, the as-coated films were post-annealed at different temperatures in air to investigate the effect of annealing temperature. Crystal structural and surface morphology of the films were measured by X-ray diffraction (XRD) and Atomic Force Microscopy (AFM). XRD patterns and AFM images indicated that the crystallinity and grain size of the films were enhanced and increased, respectively, with temperature. The tribological behavior of films was evaluated by sliding the ZnO films against a Si₃N₄ ball under 0.5 gf normal load using a reciprocating pin-on-plate tribo-tester. The wear tracks of the films were measured by AFM to quantify the wear resistance of the films. The results showed that the wear resistance of the films could be improved by the annealing process. The wear resistance of the films generally increased with annealing temperature. Specifically, the wear resistance of the films was significantly improved when the annealing temperature was higher than 550° C. The increase in the wear resistance is attributed to the increase in hardness and modulus of the film with annealing temperature.     

Modeling and simulations of nanofluids using classical molecular dynamics: Particle size and temperature effects on thermal conductivity

We use molecular dynamics simulations to investigate the thermal conductivity of argon-based nanofluid with copper nanoparticles through the Green-Kubo formalism. To describe the interaction between argon-argon atoms, we used the well-known Lennard-Jones (L-J) potential, while the copper–copper interactions are modeled using the embedded atom method (EAM) potential that takes the metallic bonding into account. The thermal conductivity of the pure argon liquid obtained in the present simulation agreed with available experimental results. In the case of nanofluid, our simulation predicted thermal conductivity values larger than those found by the existing analytical models, but in a good accordance with experimental results. This implies that our simulation is more adequate, to describe the thermal conductivity of nanofluids than the previous analytical models. The efficiency of nanofluids is improved and the thermal conductivity enhancement is appeared when the particle size and temperature increase.     

镍基625合金电子束熔覆TiC涂层表面改性研究

目的 采用电子束表面改性技术对Inconel 625镍基合金进行电子束表面合金化(EBSA)处理,制备性能良好的TiC涂层,提高Inconel 625镍基合金的表面性能。方法 采用不同的电子束扫描速度(80、100、120 mm/min)在Inconel 625镍基合金表面制备TiC涂层,使用扫描电镜(SEM)拍摄合金区横截面进行EDS能谱分析,使用电子背散射衍射仪(EBSD)对合金层进行EBSD表征分析,使用显微硬度仪测量EBSA后的表面硬度,使用摩擦磨损试验机(RTEC)测试表面耐磨性、生成摩擦曲线并拍摄磨损表面的三维形貌。结果 从宏观形貌上来看,在80 mm/min扫描速度下涂层成形质量最好。微观组织测试结果表明,随着扫描速度的增大,平均晶粒尺寸增大。显微硬度测试结果表明,随着扫描速度的增大,表面硬度呈现降低的趋势,但涂层表面硬度均高于基材硬度。当扫描速度为80 mm/min时,TiC强化颗粒较多分布在表面,其表面硬度最高,为457HB,与基材相比,表面硬度提高了1.936倍。耐磨性测试结果表明,当扫描速度为80 mm/min时,磨损体积和磨损率最低,分别为0.913 1 mm<...     

Effect of Si Content on Dynamic Recrystallization of Al-Si-Mg Alloys During Hot Extrusion

By using electron backscatter diffraction（EBSD） and transmission electron microscopy（TEM）, the effect of Si content on microstructure characteristics of three as-extruded Ale SieM g alloys was investigated. Results showed that the density of coarse Si particles played a critical role in dynamic recrystallization. Dynamic recrystallization rarely occurred in S1 alloy with less Si content; however, it happened in the Si-rich zones in S2 alloy with a medium Si content. And a mature recrystallization was observed in S3 alloy with high Si content. Although deformation was carried out at high temperature, particle-stimulated dynamic recrystallization occurred in Si-rich zones.     

Fracture mechanism of AZ31 magnesium alloy processed by equal channel angular pressing comparing three point bending test and tensile test

A commercial magnesium alloy, AZ31 in hot-rolled condition, has been processed by equal channel angular pressing (ECAP) to get microstructure modified. Uniaxial tensile tests were conducted along the rolling/extrusion direction for as-received AZ31 alloy and ECAPed AZ31 alloy. Then, three point bending fracture tests were conducted for specimens with a pre-crack perpendicular to the extruded direction. Digital image correlation (DIC) technique was adopted to determine the deformation field around the crack tip. The fracture surfaces of the failed specimens after tensile tests and fracture tests were observed by Scanning Electron Microscope (SEM). To explore the deformation mechanism, the microstructure and texture of different regions on the deformed specimens were examined through electron backscatter diffraction (EBSD). The results show ECAP process improves both the tensile elongation and fracture toughness of AZ31 alloy. Different from the slip dominated deformation mechanism in the tensile test, deformation twinning presents in the deformation zone adjacent to the crack tip in the three point bending fracture tests. The fracture surface is characterized by co-occurrence of dimple and cleavage features.     

Microstructure and mechanical behavior of ECAP processed AZ31B over a wide range of loading rates under compression and tension

In this work, a commercial magnesium alloy, AZ31B in hot-rolled condition, has been subjected to severe plastic deformation via four passes of equal channel angular pressing (ECAP) to modify its microstructure. Electron backscatter diffraction (EBSD) was used to characterize the microstructure of the as-received, ECAPed and mechanically loaded specimens. Mechanical properties of the specimens were evaluated under both compression and tension along the rolling/extrusion direction over a wide range of strain rates. The yield strength, ultimate strength and failure strain/elongation under compression and tension were compared in detail to sort out the effects of factors in terms of microstructure and loading conditions. The results show that both the as-received alloy and ECAPed alloy are nearly insensitive to strain rate under compression, and the stress–strain curves exhibit clear sigmoidal shape, pointing to dominance of mechanical twinning responsible for the plastic deformation under compression. All compressive samples fail prematurely via adiabatic shear banding followed by cracking. Significant grain size refinement is identified in the vicinity of the shear crack. Under tension, the yield strength is much higher, with strong rate dependence and much improved tensile ductility in the ECAPed specimens. Tensile ductility is even much larger than the malleability under compression. This supports the operation of 〈c + a〉 dislocations. However, ECAP lowers the yield and flow strengths of the alloy under tension. We attempted to employ a mechanistic model to provide an explanation for the experimental results of plastic deformation and failure, which is in accordance with the physical processes under tension and compression.     

Structural and magnetic properties of nickel catalyzed-tungsten oxide nanosheets synthesized using e-beam rapid thermal annealing

Nanosheets of nickel catalyzed tungsten oxide have been grown on Si (100) substrate by electron beam rapid thermal annealing (ERTA) process. The thin films of W and Ni were deposited in a conventional electron beam evaporation system under high vacuum conditions and then subjected to ERTA. Scanning electron microscopy and atomic force microscopy were used to study the systematic growth of the nanosheets. Nanosheets with a uniform thickness of 200 nm were obtained for the beam current of 9 mA with a voltage of 5 kV ERTA for 60 s. X-ray diffractograms indicate that the formation of multiple phases of nickel, nickel oxide and tungsten oxide with respect to the variation in the beam current. Vibrating sample magnetometer studies indicate that the magnetic properties of this system vary with the beam current.     

Substrate and annealing temperature effects on the optical and electrical properties of Ge20Te80 films

Ge₂₀Te₈₀ films were deposited by thermal evaporation technique onto chemically cleaned glass substrates kept at different substrate temperatures (T_sub=203, 233 and 273 K). The optical data indicated that the width of the localized states tails (E_e) increases while the optical gap (E_o) decreases with increasing the substrate and annealing temperature of the investigated films. From the electrical measurements, the activation energy for conduction and the density of localized states at the Fermi energy, N(E_F), were obtained. The effects of the substrate and annealing temperature on the width of localized states tails and on the density of localized states at the Fermi level have enhanced each other. The changes in the optical and electrical properties are correlated with the amorphous-crystalline transformations.     

Effect of high temperature annealing on the electrical performance of titanium/platinum thin films

In this study, the influence of post deposition annealing steps (PDA) on the electrical resistivity of evaporated titanium/platinum thin films on thermally oxidised silicon is investigated. Varying parameters are the impact of thermal loading with maximum temperatures up to T_PDA = 700 °C and the platinum top layer thickness ranging from 24 nm to 105 nm. The titanium based adhesive film thickness is fixed to 10 nm. Up to post deposition annealing temperatures of T_PDA = 450 °C, the film resistivity is linearly correlated with the reciprocal value of the platinum film thickness according to the size effect. Modifications in the intrinsic film stress strongly influence the electrical material parameter in this temperature regime. At T_PDA > 600 °C, diffusion of titanium into the platinum top layer and its plastic deformation dominate the electrical behaviour, both causing an increase in film resistivity above average.     

Epitaxial growth of Ni films sputter-deposited on a GaAs(001) surface covered with a MgO film

We studied the epitaxial growth of a Ni film prepared on a GaAs(001) substrate covered with a thin epitaxial MgO buffer film, assuming that this buffer film plays a key role in the epitaxial growth of the Ni film. The MgO and Ni films were deposited by radio-frequency magnetron sputtering of the MgO and Ni targets in pure Ar gas. First, a MgO film of thickness ranging from 78 to 4.4 nm was deposited on the GaAs(001) substrate at a temperature ranging from ambient temperature to 700 °C, and then, a 136-nm-thick Ni film was deposited on the MgO/GaAs substrate at a temperature range 300-500 °C. Using transmission electron microscopy and X-ray diffractometry, we showed that the MgO film grows with the epitaxial relationship MgO(001)[001]//GaAs(001)[001] on GaAs(001) at 500 °C, and that the structure of the Ni film depends on three factors: the MgO/GaAs substrate temperature, the MgO thickness, and the annealing condition of the MgO/GaAs substrate before the Ni deposition. In conclusion, we proved that the Ni film grows with the epitaxial relationship Ni(001)[001]//MgO(001)[001]//GaAs(001)[001] on MgO/GaAs with the 4.4-nm-thick MgO film when the MgO/GaAs substrate is annealed in situ at room temperature before the Ni deposition and maintained at 300 °C during the Ni deposition.     

Structural characterisation of ultra-high vacuum sublimated polycrystalline thin films of hexathiophene

Hexathiophene occupies a place of relevance in the context of organic semiconductors employed as active layers in opto-electronic devices. The knowledge of the structure of this class of materials in the film-phase is crucial for understanding and tailoring the performances of these devices. Here, thin films of hexathiophene have been deposited on silica by organic molecular beam deposition under controlled growth conditions. The structure of these films has been investigated by transmission electron diffraction compelling evidences of the presence of a structure different from the bulk phase.