Positron annihilation study of helium clustering in alpha irradiated copper

Abstract

Helium clustering in alpha irradiated copper has been investigated by positron annihilation spectroscopy. Pure copper samples have been homogeneously helium implanted using a cyclotron, yielding helium concentrations of 100 appm and 400 appm. Post-implantation positron lifetime and Doppler broadened annihilation lineshape measurements have been carried out on these Cu samples as a function of isochronal annealing temperature. An annealing stage observed in the isochronal annealing curve viz., a marked reduction in the resolved lifetime τ₂ and an increase of its intensity I ₂, is explained as due to the formation of helium bubble embryos. At higher annealing temperatures, τ₂ corresponding to helium bubbles increases and saturates while its intensity I ₂ decreases, indicating an increase in the size of the bubble with a concomitant decrease in the bubble concentration. This stage is interpreted to be the bubble growth stage. From an analysis of positron lifetime parameters in the growth stage, helium stom density, bubble size and bubble concentration have been deduced at various annealing temperatures. The bubble characteristics are found to be affected by the helium dose. The present results on direct helium implanted Cu are compared with those of our earlier study on n-irradiated Cu-B, where helium was introduced using ¹⁰B(n, α)⁷ Li reaction.     

Pseudo-potential caculations of positron annihilation rates in bubbles of helium contained in the metals Mg,Ag and Au

Abstract

A pseudo-potential technique has been applied to calculate the annihilation rates for positrons in bubbles of helium gas in gold and silver. The positron pseudo-wavefunction in each case was found to be in a surface state of the metal, the exact form of which displayed a slight dependance on the density of the helium gas. The annihilation rate of the positron was the sum of a nearly constant surface rate and a strongly density dependant annihilation rate with the helium electrons. There is a trend for annihilation with the helium to be greater in metals with low free electron densities, the helium in such metals resting closer to the metal surface thus increasing the overlap of the positron wavefunction with the helium.     

Alpha particle detection by the diacel solid state track detector

The characteristics of diacel plastic track detector are investigated for the detection of alpha particles. The influence of different radiations viz. electrons, gamma rays, ultraviolet rays, infrared rays and neutrons on the detector has also been studied.     

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.     

正电子湮没谱和光致发光谱研究掺锌GaSb质子辐照缺陷

用正电子湮没谱和光致发光谱研究了质子辐照后掺锌GaSb中的缺陷.通过分析正电子的缺陷寿命τ₂及强度I₂的变化发现,在高能质子的辐照下产生了双空位缺陷V_GaV_Sb,可能同时产生了小的空位团.正电子平均寿命τ_av和S参数随着质子辐照剂量的变化也证明了这一结论.通过分析不同质子辐照剂量下掺锌GaS     

用正电子研究NaCl在NaY沸石上的固溶过程

用正电子湮没谱学研究NaCl与NaY沸石机械混合后, NaCl在NaY中的固溶扩散过程.分别测量不同质量比的NaCl/NaY［(1—20)%］经500℃烘烤1h，NaCl/NaY(15%)经不同温度烘烤1h,以及NaCl/NaY(15%)经500℃烘烤不同时间后的正电子寿命谱.所有寿命谱都出现了5个寿命分量, 其中第3，4，5寿命分别与β笼、超笼及沸石微粒界面空洞的大小和数量相关.实验表明正电子湮没谱学能敏感地表征NaCl在NaY中的固溶扩散过程. 关键词： 正电子湮没谱学 氯化钠 沸石     

JRQ and JPA irradiated and annealed reactor pressure vessel steels studied by positron annihilation

The paper is focused on a comprehensive study of JRQ and JPA reactor pressure vessel steels from the positron annihilation lifetime spectroscopy (PALS) point of view. Based on our more than 20 years’ experience with characterization of irradiated reactor steels, we confirmed that defects after irradiation start to grow and/or merge into bigger clusters. Experimental results shown that JPA steel is more sensitive to the creation of irradiation-induced defects than JRQ steel. It is most probably due to high copper content (0.29?wt.% in JPA) and copper precipitation has a major impact on neutron-induced defect creation at the beginning of the irradiation. Based on current PALS results, no large vacancy clusters were formed during irradiation, which could cause dangerous embrittlement concerning operation safety of nuclear power plant. The combined PALS, small angle neutron scattering and atomic probe tomography studies support the model for JRQ and JPA steels describing the structure of irradiation-induced clusters as agglomerations of vacancy clusters (consisting of 2–6 vacancies each) and are separated from each other by a distribution of atoms.     

Hydrogen behaviour in electron-irradiated titanium alloys studied by positron annihilation method

Measurements of angular distribution of annihilation photons are applied to investigations of hydrogen behavior in annealed, plastically deformed, and irradiated titanium alloys. It is shown that hydrogen interaction with materials becomes more intensive in presence of structural imperfections of deformational and radiation origin. Probable mechanisms of hydrogen interaction with deformational and radiation defects are discussed.     

利用正电子湮没技术研究钾掺杂钨合金中的缺陷

钨合金中钾的掺杂会引入大量的缺陷,如尺寸几十纳米的钾泡、高密度的位错以及微米量级的晶粒带来的晶界等,这些缺陷的浓度和分布直接影响合金的服役性能.本文运用正电子湮没谱学方法研究钾掺杂钨合金中的缺陷信息,首先模拟计算了合金中各种缺陷的正电子湮没寿命,发现钾的嵌入对空位团、位错、晶界等缺陷的寿命影响很小;然后测量了不同钾含量掺杂钨合金样品的正电子湮没寿命谱,建立三态捕获模型,发现样品中有高的位错密度和低的空位团簇浓度,验证了钾对位错的钉扎作用,阐述了在钾泡形成初期是钾元素与空位团簇结合并逐渐长大的过程;最后使用慢正电子多普勒展宽谱技术表征了样品中缺陷随深度的均匀分布和大量存在,通过扩散长度的比较肯定了钾泡、晶界等缺陷的存在.     

Positronium annihilation in silica aerogel studied by a positron age-momentum correlation technique

A high-performance positron age-momentum correlation (AMOC) spectrometer was newly developed.The counting rate is increased up to 200 cps much larger than the value 20 cps reported by other international groups.And at the same time,the time resolution still keeps at the international level of 220 ps.Furthermore,positronium (Ps) annihilation in silica aerogel was investigated by AMOC,which indicates:(1) Ps annihilation between the grains dominantly undergoes pick-off process and spin conversion from o-Ps to p-Ps;(2) Annealing below 400 ℃ changes the grain surface conditions,i.e.the desorption of hydrogen and the decrease of the defect centers concentration.     

Positronium annihilation in silica aerogel studied by a positron age-momentum correlation technique

A high-performance positron age-momentum correlation (AMOC) spectrometer was newly developed. The counting rate is increased up to 200 cps much larger than the value 20~cps reported by other international groups. And at the same time, the time resolution still keeps at the international level of 220 ps. Furthermore, positronium (Ps) annihilation in silica aerogel was investigated by AMOC, which indicates: (1) Ps annihilation between the grains dominantly undergoes pick-off process and spin conversion from o-Ps to p-Ps; (2) Annealing below 400 ℃ changes the grain surface conditions, i. e. the desorption of hydrogen and the decrease of the defect centers concentration.     

Correlation between ferromagnetism and defects in MgO nanocrystals studied by positron annihilation

High purity MgO nanopowders were pressed into pellets and annealed in air from 100 to 1400 °C. Variation of the microstructures was investigated by X-ray diffraction and positron annihilation spectroscopy. Annealing induces an increase in the MgO grain size from 27 to 60 nm with temperature increasing up to 1400 °C. Positron annihilation measurements reveal vacancy defects including Mg vacancies, vacancy clusters, microvoids and large pores in the grain boundary region. Rapid recovery of Mg monovacancies and vacancy clusters was observed after annealing above 1200 °C. Room temperature ferromagnetism was observed for MgO nanocrystals annealed at 100, 700, and 1000 °C. However, after 1400 °C annealing, MgO nanocrystals turn into diamagnetic. Our results suggest that the room temperature ferromagnetism in MgO nanocrystals might originate from the interfacial defects.     

Free-volume changes at nanoscale in doped polyacrylic acid studied by positron annihilation spectroscopy

Polyacrylic acid (PAA) doped with carbon black (CB), chromium oxide (Cr₂O₃) and cupferron with different wt% (0.25%, 0.50%, 0.75%, and 1%) was studied using positron annihilation lifetime (PAL) technique and Doppler broadening of annihilation radiation (DBAR). Ortho-positronium lifetime components (τ₃ and I₃) were used to estimate the nanoscale free-volume hole sizes (V_f) and its fractions (f). It was found that the hole size V_f and its fractions f as well as S-parameters decreased at high value of doping concentration due to dopants-polymer formation. These results are supported by a significant narrowing in the nanoscale free-volume hole size distributions.

The correlation between positron annihilation parameters and electric conductivity are discussed.     

Identification of pore size in porous SiO2 thin film by positron annihilation

Positron annihilation lifetime and Doppler broadening of annihilation line techniques have been used to obtain information about the small pore structure and size of porous SiO2 thin film produced by sputtered Al-Si thin film and etched Al-Si thin film. The film is prepared by an Al/Si 75：25 at.-% （A175Si25） target with the radiofrequency （RF） power of 66 W at room temperature. A 5 wt.-% phosphoric acid solution is used to etch the Al cylinders. All the A1 cylinders dissolved in the solution after 15 h at room temperature, and the sample is subsequently rinsed in pure water. In this way, the porous SiO2 on the Si substrate is produced. From our results, the values of all lifetime components in the spectra of Al-Si thin film are less than 1 ns, but the value of one of the lifetime components in the spectra of porous SiO2 thin film is τ = 7.80 ns. With these values of lifetime, RTE （Rectangular Pore Extension） model has been used to analyze the pore size.     

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.     

Identification of pore size in porous SiO2 thin film by positron annihilation

Positron annihilation lifetime and Doppler broadening of annihilation line techniques have been used to obtain information about the small pore structure and size of porous SiO2 thin film produced by sputtered A1-Si thin film and etched Al-Si thin film. The film is prepared by an Al/Si 75:25 at.-% (A175Si25) target with the radiofrequency (RF) power of 66 W at room temperature. A 5 wt.-% phosphoric acid solution is used to etch the A1 cylinders. All the Al cylinders dissolved in the solution after 15 h at room temperature, and the sample is subsequently rinsed in pure water. In this way, the porous SiO2 on the Si substrate is produced. From our results, the values of all lifetime components in the spectra of Al-Si thin film are less than 1 ns, but the value of one of the lifetime components in the spectra of porous SiO2 thin film is T = 7.80 ns. With these values of lifetime, RTE (Rectangular Pore Extension) model has been used to analyze the pore size.     

用正电子湮没多普勒增宽谱测量金属中电子的费米能级

高校中不少实验室具有半导体探头能谱仪,可扩展用作正电子湮没多普勒增宽谱仪,并测量金属中电子的费米能级     

Free volumes in bulk nanocrystalline metals studied by the complementary techniques of positron annihilation and dilatometry

Free-volume type defects, such as vacancies, vacancy-agglomerates, dislocations, and grain boundaries represent a key parameter in the properties of ultrafine-grained and nanocrystalline materials. Such free-volume type defects are introduced in high excess concentration during the processes of structural refinement by severe plastic deformation. The direct method of time-differential dilatometry is applied in the present work to determine the total amount and the kinetics of free volume by measuring the irreversible length change upon annealing of bulk nanocrystalline metals (Fe, Cu, Ni) prepared by high-pressure torsion (HPT). In the case of HPT-deformed Ni and Cu, distinct substages of the length change upon linear heating occur due to the loss of grain boundaries in the wake of crystallite growth. The data on dilatometric length change can be directly related to the fast annealing of free-volume type defects studied by in situ Doppler broadening measurements performed at the high-intensity positron beam of the FRM II (Garching, Munich, Germany).     

Helium/hydrogen synergistic effect in reduced activation ferritic/martensitic steel investigated by slow positron beam

Here, we investigated the irradiation defect in reduced activation ferritic/martensitic steels by slow positron beam. Three ion-irradiation experiments were carried out: (i) He²⁺ irradiation, (ii) H⁺ irradiation and (iii) He²⁺ irradiation followed by H⁺ irradiation, at temperature 450?°C. The presences of vacancy defects, represented by ?S_He+H parameter, induced by sequential irradiations was larger than the sum of defects, ?S_He parameter + ?S_H parameter, caused by single He ions and single H ions. The synergistic effect of He and H was confirmed clearly from the perspective of positron annihilation spectroscopy.     

中频磁脉冲处理Fe52Co34HfTB6Cu1非晶合金的正电子湮没研究

对熔体急冷法制备的非晶合金Fe52Co34HfTB6Cu1进行了不同频率的中频磁脉冲处理,用透射电子显微镜、穆斯堡尔谱、正电子湮没寿命谱等方法研究了处理前后试样的微观结构及结构缺陷变化．结果表明,经中频磁脉冲处理后,样品发生了部分纳米晶化,晶化量随磁脉冲频率增加而增加,当磁脉冲频率为2000Hz时,晶化量达33．1％：在淬态非晶样品中,正电子在类单空位中的湮没寿命t1为150．5ps,强度,1为77．7％,在微孔洞中的湮没寿命仡为349．7ps,强度I2为22．3％;随磁脉冲频率的增加,t1,t2值呈现减小的变化趋势,与淬态非晶相比,I1有所增加,如下降,t1,t2的平均值亍大幅降低．