Study of the effect of annealing on defects in Fe-Mn-Si-Cr-Ni-C alloy by slow positron beam

FeMnSi shape memory alloys (SMAs) have received much attention as one-way SMAs due to their cost-effectiveness. Variable-energy (0-30 keV) positron beam studies have been carried out on a Fe-Mn-Si-Cr-Ni-C alloy with different degrees of deformation. Doppler broadening profiles of the positron annihilation as a function of incident positron energy were shown to be quite sensitive to defects introduced by deformation. The variation of the nature and the concentration of defects are studied as a function of isochronal annealing temperature. These results are correlated with the data measured with the positron annihilation lifetime spectroscopy (PALS). The positron annihilation results are compared to XRD and optical microscopy (OM).     

Characterisation of atomic-scale defects in ODS ferritic alloys by positron annihilation

The vacancy-type defects and their local chemical environment in different ODS alloys produced in the USA (14YWT), China (K5) and Russia (ODS EP-450) are studied. The Angular Correlation of Annihilation Radiation (ACAR), which is one of the positron annihilation spectroscopy method, was used. It was shown that in all alloys, except 14YWT, the dominant type of positron traps are vacancy-like defects, localised in matrix or associated with dislocations and/or interfaces of the incoherent particles. In the case of 14YWT alloy, which contains Y–Ti–O nanoclusters of a high density, the positrons confine and annihilate at O-vacancy pairs or complexes within nanoclusters. It is testified by enhanced electron density in annihilation sites and neighbourhood of Ti and Y atoms. These results, obtained by the ACAR method, indicate that the vacancies play an essential role in the formation of nanoclusters in ODS 14YWT alloy as it was theoretical predicted by first-principle calculations.     

Fe-Ni合金马氏体相变缺陷的正电子湮没研究

本文中用正电子湮没技术研究了Fe-Ni系合金的马氏体相变。实验结果表明,含镍量28.22—31.30wt％的六种退火态合金,正相变后,产生了大量的缺陷,使正电子湮没平均寿命及多普勒加宽线型参数S值分别约增加30％和20％。对28.93wt％Ni和31.30wt％Ni两种马氏体亚结构不同的合金,观测了正电子湮没参数与处理温度之间的关系,发现:缺陷主要产生在爆发马氏体形成阶段;在等时退火曲线上形成两个明显的台阶,是由于空位和位错恢复引起的。 关键词：     

Application of positron annihilation spectroscopy on the ion implantation damaged Fe-Cr alloys

Four different Fe-Cr binary alloys with Cr content 2.5-11 wt% were studied in details using various methods. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were applied to obtain basic information, required for standard positron annihilation lifetime spectroscopy (PALS) spectra analysis. Additionally, PALS measurements were performed on as-received state as well as on helium implanted specimens. The He implantation was proposed for simulation of radiation damage and obtain high doses even in near surface areas (up to 1 μm). The implantation was based on the SRIM code simulation and next DPA calculations. Final concentration of vacancy type defects were calculated for 250 keV He²⁺ beam and the maximum was determined in 600 μm depth. Such specimens are very suitable for positron beam study of vacancy type defect mobility as a result of thermal treatment, which will be performed simultaneously in the future.     

Behavior of structure defects and hydrogen in neutron-irradiated stainless steels studied by positron annihilation method

Measurements of angular distributions of annihilation photons are applied to investigating structural defects and hydrogen behavior in annealed, plastically deformed, and irradiated stainless steels. It is determined that the whole cycle of investigations performed by positron diagnostics helped in tracing the formation and evolution of the defect structure and hydrogen behavior in different kinds of steels being subjected to complex physical–mechanical influences such as plastic deformation, hydrogenation and irradiation by fission neutrons. The high sensitivity of the electron–positron annihilation method allowed understanding even of details of the changes of the crystalline structure of multi-component materials.     

The role of quenched‐in vacancies for the decomposition of aluminium alloys

The very early stages of decomposition during room temperature storage, i.e. just a few minutes after quenching, are investigated by positron annihilation lifetime spectroscopy for both an AlMgSi alloy and an AlCuMg alloy. It turns out that by freezing the decomposition kinetics during measurements we can detect vacancy–solute atom pairs. The formation of larger solute clusters with structural vacancies is seen by an increase of the mean positron lifetime in the course of storage at room temperature (RT). Earlier findings concerning aging at RT were unable to discover this effect. The detected changes are interpreted in terms of cluster formation. Thus we show that positron annihilation spectroscopy (PAS) is one of the very few methods to access early stages of decomposition in metallic alloys. Moreover, the lower limit of the concentration of quenched‐in vacancy‐like defects is calculated to be at least 2 × 10^–5 per atom. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Point-defect production in arsenic-doped silicon studied with variable-energy positrons

Silicon epilayers grown by molecular beam epitaxy and doped in-situ using low-energy implantation were examined using a variable-energy positron beam. The samples had been previously characterized using electrical measurements, ion channeling, SIMS, and electron microscopy. The positron results show that defects have been created in layers grown at 460°C and in the highly doped layers grown at 700°C. The assignment of defect structures is difficult at present, but is consistent with the formation of As clusters or Asvacancy complexes.     

Electrostatic Nonlinear Structures in Dissipative Electron--Positron--Ion Quantum Plasmas

Low frequency （in comparison to ion plasma frequency） ion-acoustic shocks and solitons in superdense electronpositron-ion quantum plasmas are studied. The quantum hydrodynamic model is used incorporating quantum Bohm forces and Fermi-Dirac statistical corrections to derive the deformed Korteweg de Vries-Burgers （dKdVB） equation in weakly nonlinear limit. The travelling wave solution of dKdVB equation is presented and results are discussed in different limits. It is found that shock height increases with increase of quantum pressure, positron concentration and dissipation. Further, it is seen that the width of soliton decreases with increase of quantum pressure     

New design of the CDB-spectrometer at NEPOMUC for T-dependent defect spectroscopy in Mg

Crystal defects in magnesium and magnesium-based alloys like AZ31 are of major interest for the understanding of their macroscopic properties. Coincident Doppler broadening spectroscopy with positrons (CDBS) is a well-established technique to investigate lattice defects and their chemical surrounding in solids. However, Mg and its alloys are demanding materials for positron spectroscopy, since the trapping rate in Mg is low and the trapping sites are shallow. In order to increase the trapping rate, the CDBS-facility at the high intense positron beam NEPOMUC is currently redesigned and improved with a cryostat for sample cooling. Furthermore, the recently installed remoderator provides a beam energy between 20 and 200 eV. On the contrary to the previous beam energy of 1 keV, the beam is therefore no longer non-adiabatically released from the magnetic field at the grounded field termination. Hence it is necessary to construct an insulated field termination where voltages up to 5 kV can be applied.     

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.     

An Experimental Study of Mg Aggregation in AA5754 Alloys by Positron Annihilation Spectroscopy

Defects in an AA5754 （Al-3.0%Mg） alloy are investigated by coincidence Doppler broadening spectroscopy and positron lifetime spectroscopy. The results indicate enhancement of positron trapping by Mg atoms in this Al-Mg alloy after quenching treatment at 623K, which may be due to the formation of vacancy-Mg complexes or the aggregation of Mg near the vacancy sites. It is speculated that the aggregation of Mg atoms in the moderate temperature range is responsible for cracking in spot welding of AA5754 alloys.     

Positron annihilation in electron-irradiated n-type gap crystals

Abstract

The defects in n-GaP crystals irradiated by 2.3 MeV electrons up to 1 × 10¹⁹ cm^?2 at RT were studied by means of positron annihilation (angular correlation) and electrical property measurements. It was found that positrons are trapped in some radiation-induced vacancy-type defects (acceptors) but that the effect saturates at high electron fluences (D1 × 10¹⁸ cm^?2). The trapping rate in irradiated samples increases with temperature in the range 77–300 K. Post-irradiation isochronal annealing reveals the positron traps clustering at about 200–280°C. All positron sensitive radiation-induced defects disappear upon annealing up to 500°C.     

Surface phase transformation induced by the dezincification of a beta Cu-Zn alloy on highly deformed systems

When Cu-Zn alloys are annealed under dynamical vacuum the Zn component evaporates. The process is called dezincification. This paper presents the results of the dezincification of highly mechanically deformed surfaces of samples initially in the beta (bcc) phase by a combination of in situ optical microscopy observations together with TEM measurements. It is shown that grinding lines remaining from the sample preparation process act as nucleation centers for the alpha (fcc) phase. Under this surface preparation conditions the new fcc phase nucleates with a different geometry than the one reported in previous papers in which surfaces were finished by electropolishing. In the present case, we observe individual fcc precipitates with a well defined geometry. The typical size of precipitates is in the micron range, and depends on the dezincification parameters: final temperature, dezincification time and prior surface preparation. TEM observations show that the fcc precipitates contain a large density of defects, mainly dislocations and twin boundaries.     

铁冷轧形变以及热处理对形变缺陷的影响

采用常用冷轧设备对铁进行冷轧引入形变缺陷。研究形变量和温度对形变缺陷的影响。形变样品中的微观缺陷、物相结构和形貌分别使用正电子湮没技术（PAT）、X射线衍射仪（XRD）和透射电子显微镜（TEM）进行表征分析。对经过673 K热处理的形变样品前后进行XRD测试,结果显示,随着形变量的增加,样品中晶面方向（200）具有择优生长趋势,673 K热处理后,择优趋势更加明显,同时晶粒的尺寸也增大。利用正电子湮没寿命谱和多普勒展宽能谱对样品中形变缺陷的热力学稳定性进行研究,发现形变引入的空位型缺陷约在673 K回复完毕,723 K后位错缺陷开始回复。The pure iron was cold rolled with the thickness reduction from 0% to 75%. The microstructure defects, crystallographic structure and morphology of deformed specimens were characterized by positron annihilation technique (PAT), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD results show that the intensity of (200) increased with increasing deformation, 673 K heat-treatment promote the preference of (200) and the grain size of (200) was increased. The PAT results show that the vacancy type defect was annihilated at 673 K and the dislocation type defects start to annihilate at 723 K.     

Lattice defects in ion-implanted aluminium studied by means of perturbed angular correlations

Migration and clustering of lattice defects after implantation of¹¹¹In in Al and subsequent annealing at temperatures in the range from 80 to 800 K were investigated applying the DPAC technique. The effects of implantation dose, implantation temperature, laser irradiation, and plastic deformation were studied. The measurements on plastically deformed Al were complemented by positron lifetime measurements. We observed four In-defect clusters that can be flagged by well-defined hyperfine interaction parameters, and we determined their symmetry properties by using single-crystal samples. Important conclusions are: (i) monovacancies are not trapped by In-atoms, (ii) small In-defect clusters are formed by direct trapping of divacancies and/or trivacancies, and (iii) extended In-defect clusters are very stable and anneal in the temperature range 600–700 K. Consequences for the interpretation of other measurements on dilute Al(In) alloys are discussed.On leave from Tata Institute of Fundamental Research, Homi Bhabha Road, Bombay 400 005, India.     

铝纳米晶的正电子湮没研究

采用自悬浮定向流-真空热压法,在不同压强下制得铝纳米晶材料,并利用X射线衍射(XRD)和正电子湮没寿命谱(PALS)分析手段对铝纳米晶的结构和微观缺陷进行表征.XRD分析表明:所制备的铝纳米晶的晶粒度为48 nm.PALS分析表明:铝纳米晶的微观缺陷主要为类空位以及空位团,而微孔洞很少;短寿命τ1,中间寿命τ2以及其对应的强度I1,I2随压强变化而呈现阶段性变化;压制压强(P)低于0.39 GPa时制得的纳米晶空位团随压强的增加而逐渐转变为类空位;0.39 GPa P 0.72 GPa时,各类缺陷发生消除;P 0.72 GPa时,各类缺陷进一步发生消除.随压强的提高,铝纳米晶的密度增加,其显微硬度也明显增高.     

Early stage ageing effects and shallow positron traps in Al–Mg–Si alloys

Room temperature ageing, so-called natural ageing, of Al–Mg–Si alloys has a subtle but striking influence on the mechanical properties achievable by subsequent ageing at more elevated temperatures. Though strongly debated, different clustering processes are generally accepted to give rise to this effect. Using temperature-dependent positron lifetime measurements of naturally aged Al–Mg–Si alloys, it is shown that in the early stages of ageing, small clusters of alloying atoms without embedded vacancies take part in the decomposition process. These clusters serve as shallow positron traps with a binding energy of about 55(10) meV, grow in the course of natural ageing and transform to deep positron traps with binding energies well above thermal energies. Thus, results of positron annihilation spectroscopy techniques need to be interpreted carefully with respect to the microstructure of age-hardenable Al alloys. Moreover, it is shown that a simple approach to bind positron states using a three-dimensional potential well and (bulk) positron affinities cannot explain the present findings.     

Positron annihilation studies on the migration of deformation induced vacancies in stainless steel AISI 316 L

Positron lifetime measurements were carried out at room temperature before and after isochronous annealing of cylindrical, machined fatigue specimens and of round slabs of austenitic stainless steel AISI 316 L deformed in compression. Annealing experiments are evaluated in terms of vacancy migration and sinking to grain boundaries and dislocations. The model assumes spherical grains with a homogeneous initial distribution of vacancies. A vacancy migration enthalpy of H^M _V=(0.9±0.15) eV was found. It is concluded that positron trapping at dislocation lines does not significantly contribute to positron lifetime measurements at room temperature and that single vacancies are the dominating positron traps. Positron annihilation depth profiling on cross-sectional areas prepared from machined specimens using a positron microprobe with 10 μm spatial resolution shows that machining of cylindrical specimens creates vacancies up to 5 mm below the surface. Received: 11 August 2000 / Accepted: 13 November 2000 / Published online: 28 February 2001     

Surface and bulk investigations at the high intensity positron beam facility NEPOMUC

The NEutron-induced POsitron source MUniCh (NEPOMUC) at the research reactor FRM II delivers a low-energy positron beam (E = 15-1000 eV) of high intensity in the range between 4 × 10⁷ and 5 × 10⁸ moderated positrons per second. At present four experimental facilities are in operation at NEPOMUC: a coincident Doppler-broadening spectrometer (CDBS) for defect spectroscopy and investigations of the chemical vicinity of defects, a positron annihilation-induced Auger-electron spectrometer (PAES) for surface studies and an apparatus for the production of the negatively charged positronium ion Ps⁻. Recently, the pulsed low-energy positron system (PLEPS) has been connected to the NEPOMUC beam line, and first positron lifetime spectra were recorded within short measurement times. A positron remoderation unit which is operated with a tungsten single crystal in back reflection geometry has been implemented in order to improve the beam brilliance. An overview of NEPOMUC's status, experimental results and recent developments at the running spectrometers are presented.     

形变充氢多晶纯钴中缺陷的正电子湮没研究

用正电子寿命和多普勒线形参数测量技术,研究了形变和形变充氢多晶钴试样的缺陷性质及其回复行为。观察到形变样品阴极充氢后,氢致缺陷为一定量的位错和空位以及少量的空位团。没有观察到微空洞和微裂纹的产生。单空位的回复温度范围为73—260℃,位错和空位团的退火发生在350—670℃温度范围。测得空位的迁移激活能为E_v^m=1.09±0.07eV。 关键词：