Ion Beam Analysis of the Annealing Behavior of Helium in Ti Films

We present a theoretical calculation finding that a spectrum from ion beam analysis will change at different stopping cross sections. This is more visible at a deeper place in the sample. Helium-contained Ti films annealed at different temperatures are prepared to gain different stopping cross sections whereby the stopping cross section will change with the helium phase states and the pressure of helium bubbles. Then ion beam analysis is used to measure the concentration of helium. It is found that the concentration curve rises greatly after the sample is annealed at 673K which reflects the increasing size of the helium bubble. The results axe consistent with that of positron annihilation radiation spectra which are performed by using a changeable energy positron beam.     

Evolution,migration and clustering of helium-vacancy complexes in RAFM steel- depth resolved positron annihilation Doppler broadening study

Indian Reduced Activation Ferritic Martensitic steel is implanted with 130 keV helium ions to a fluence of 5 × 10¹⁴ and 1 × 10¹⁶ ions/cm² and investigated using positron annihilation spectroscopy. The samples were characterised by defect sensitive S and W-parameters using depth resolved slow positron beam. A dose dependency is observed in the nucleation and growth of helium bubbles with annealing temperature. An experimental evidence for the migration of smaller helium-vacancy complexes is observed via the variation in thickness/width of irradiated layer with temperature. The S–W plot clearly shows the regions corresponding to defect annealing, bubble nucleation and growth.     

Helium bubbles in neutron-irradiated copper-boron studied by positron annihilation

The influence of helium, introduced by the ¹⁰B(n, α)⁷Li reaction, on the evolution of defect structure in copper containing a few hundred ppm boron has been studied by detailed positron lifetime and two-photon angular correlation measurements, supplemented by TEM studies. In the as-irradiated state of Cu-B, two lifetime components have been resolved. The shorter lifetime, τ₁, = 167 ps of 97% intensity, has been understood as due to positron trapping at small helium-vacancy complexes, while the longer lifetime τ₂ = 450 ps of 3% intensity is explained as due to helium-free voids. Marked changes in the annihilation characteristics observed at 670 K are interpreted in terms of the nucleation of microbubbles, controlled by thermally activated helium migration to vacancy traps. Corroborative evidence for the onset of helium clustering is obtained from the change in the average size of positron traps as deduced from the smearing of the measured angular correlation spectra. Helium bubbles and helium-free voids coexisting in the system have been distinguished by a three-component analysis of the lifetime spectra. Bubbles are found to be stable beyond the temperature of dissociation of voids. The size and concentration of bubbles, determined independently by TEM measurements, are in accordance with the positron annihilation results in the growth stage. The observed positron lifetime at higher annealing temperatures has been analysed by relating the annihilation rate to helium atom density and helium pressures in bubbles evaluated. These pressures are in satisfactory agreement with the estimates of equilibrium pressures, leading to the conclusion that bubble relaxation occurs by the mechanism of thermal vacancy condensation.     

In-situ TEM observation of the evolution of helium bubbles in Mo during He+ irradiation and post-irradiation annealing

The evolution of helium bubbles in purity Mo was investigated by in-situ transmission electron microscopy (TEM) during 30 keV He⁺ irradiation (at 673 K and 1173 K) and post-irradiation annealing (after 30 keV He⁺ irradiation with the fluence of 5.74×10¹⁶ He⁺/cm² at 673 K). Both He⁺ irradiation and subsequently annealing induced the initiation, aggregation, and growth of helium bubbles. Temperature had a significant effect on the initiation and evolution of helium bubbles. The higher the irradiation temperature was, the larger the bubble size at the same irradiation fluence would be. At 1173 K irradiation, helium bubbles nucleated and grew preferentially at grain boundaries and showed super large size, which would induce the formation of microcracks. At the same time, the geometry of helium bubbles changed from sphericity to polyhedron. The polyhedral bubbles preferred to grow in the shape bounded by {100} planes. After statistical analysis of the characteristic parameters of helium bubbles, the functions between the average size, number density of helium bubbles, swelling rate and irradiation damage were obtained. Meanwhile, an empirical formula for calculating the size of helium bubbles during the annealing was also provided.     

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.     

Radiation defects induced by helium implantation in gold-based alloys investigated by positron annihilation spectroscopy

The formation of gas bubbles in metallic materials may result in drastic degradation of in-service properties. In order to investigate this effect in high density and medium-low melting temperature (T _M) alloys, positron annihilation spectroscopy measurements were performed on helium-implanted gold–silver solid solutions after isochronal annealing treatments. Three recovery stages are observed, attributed to the migration and elimination of defects not stabilized by helium atoms, helium bubble nucleation and bubble growth. Similarities with other metals are found for the recovery stages involving bubble nucleation and growth processes. Lifetime measurements indicate that He implantation leads to the formation of small and over-pressurized bubbles that generate internal stresses in the material. A comprehensive picture is drawn for possible mechanisms of helium bubble evolution. Two values of activation energy (0.26 and 0.53 eV) are determined below and above 0.7T _M, respectively, from the variation of the helium bubble radius during the bubble growth stage. The migration and coalescence mechanism, which accounts for these very low activation energies, controls the helium bubble growth.     

Vacancy trapping and helium decoration in Sb ion-implanted tungsten studied by Mössbauer spectroscopy

Mössbauer effect measurements have been performed using sources of¹¹⁹Sb implanted in W without and with post-implanted helium. Each of the sources was subjected to an isochronal annealing sequence in order to study vacancy trapping, helium decoration and recovery of damage. Four sites have been identified for Sb implanted in tungsten; one of these corresponds with substitutional Sb atoms, two others are assigned to Sb atoms associated with vacancies, while the last one can be either vacancy or impurity associated. The development of site occupation as a function of annealing temperature is in accordance with the one-interstitial model. Injection of 2·10¹⁶ He/cm² leads to nucleation of helium bubbles. Helium atoms that are released from these bubbles at about 1300 K are retrapped by Sb atoms to form new bubbles.     

高密度氦相变的分子动力学研究

采用分子动力学方法结合对关联函数分析计算了0–1000 K范围内氦的固–液相变曲线, 与实验数据的对比显示, 在0–500 K之间与实验数据符合很好, 500 K以上还没有相应的实验数据. 另外, 计算了钛金属中不同尺寸氦泡的压强, 并与高密度氦的固–液相变曲线进行了对比. 结果显示, 在低温条件下, 随着温度的降低, 钛晶体中可能会出现固态氦泡; 在300 K以上不会存在固态氦泡.     

Helium implanted CuHf as studied by TDPAC and positron lifetime measurements

¹⁸¹Ta time differential perturbed angular correlation (TDPAC) and positron lifetime measurements were carried out on homogeneously α-implanted CuHf samples. TDPAC measurements indicate the trapping of vacancy clusters and helium associated defect complexes by Hf atoms. The presence of helium-vacancy complexes and helium stabilised voids has been identified by positron lifetime measurements. Further the nucleation and growth stages of helium bubbles have been identified. TDPAC and positron lifetime measurements indicate that Hf atoms act as heterogeneous nucleating centers for helium bubbles. Hf atoms are found to suppress the bubble growth in CuHf as indicated by the results of positron lifetime measurements.     

The density of helium in bubbles in implanted materials: Results from VUV absorption and eel spectroscopy

Abstract

The novel application of vacuum ultra-violet absorption spectroscopy and electron energy loss spectroscopy to helium bubbles in metals is presented. These measurements, carried out on thin aluminium films containing different concentrations of helium and various bubble size distributions, were aimed at determining the density (and thus pressure) of helium in bubbles by observing the shift and broadening of the IS-2P transition in the helium. The data coupled with a theoretical model developed by the authors (see following paper) indicate densities as high as 10²³ He cm^?3 for specimens containing small bubbles. Data are also presented on the effect that annealing and cooling have on these spectra. The annealing experiments give rise to fairly complex changes in absorption peak structure but with a general shift towards the unperturbed resonance line. The cooling experiment gives rise to a further shift and a narrowing of the absorption spectrum on cooling to 77 K which is tentatively identified as the liquid/solid transition in the helium. Finally, fluorescence spectrum of an Al/He specimen excited with low energy electrons is presented.     

Gentle quantitative measurement of helium density in nanobubbles in silicon by spectrum imaging

We propose an original method for the determination of the physical properties of nanometer sized helium bubbles using spectrum imaging in an energy-filtered transmission electron microscope. Helium bubbles synthesized by high fluence implantation and thermal annealing in silicon are investigated. The acquisition parameters are determined to optimize both signal/noise ratio and time. The limitations to the extent of observable areas on a typical sample are explained. The necessary data correction and helium K-edge position measurement procedures are detailed and the accuracy of the method is discussed. Finally helium density maps are obtained and discussed.     

Evolution of helium bubbles in nickel-based alloy by post-implantation annealing

Nickel-based alloys have been considered as candidate structural materials used in generation IV nuclear reactors serving at high temperatures. In the present study, alloy 617 was irradiated with 180-keV helium ions to a fluence of 3.6×10¹⁷ ions/cm² at room temperature. Throughout the cross-section transmission electron microscopy (TEM) image, numerous over-pressurized helium bubbles in spherical shape are observed with the actual concentration profile a little deeper than the SRIM predicted result. Post-implantation annealing was conducted at 700 ℃ for 2 h to investigate the bubble evolution. The long-range migration of helium bubbles occurred during the annealing process, which makes the bubbles of the peak region transform into a faceted shape as well. Then the coarsening mechanism of helium bubbles at different depths is discussed and related to the migration and coalescence (MC) mechanism. With the diffusion of nickel atoms slowed down by the alloy elements, the migration and coalescence of bubbles are suppressed in alloy 617, leading to a better helium irradiation resistance.     

Surface damage and topography of erbium metal films implanted with helium to high fluences

Topographical and expansion effects which occur as a result of implanting erbium thin films with helium up to fluences of 1.5 × 10¹⁸ He⁺/cm² are described. There exists an inverse relationship between critical dose and annealing temperature with respect to the formation of surface bubbles. Post implantation annealing at or below 400°C is found to strongly reduce implantation induced expansion for doses less than 3.5 × 10¹⁷ He⁺/cm², but is observed to result in increased expansion above this dose. At temperatures above 400°C, expansion is increased for all doses investigated. Details of bubble development in the implanted layer are discussed and the manner in which surface bubbles develop from enlarged subsurface bubbles is illustrated.     

Study of He-induced nano-cavities as sinks of oxygen for forming silicon-on-insulator

In the present work, a Cz-Silicon wafer is implanted with helium ions to produce a buried porous layer, and then thermally annealed in a dry oxygen atmosphere to make oxygen transport into the cavities. The formation of the buried oxide layer in the case of internal oxidation （ITOX） of the buried porous layer of cavities in the silicon sample is studied by positron beam annihilation （PBA）. The cavities are formed by 15 keV He implantation at a fluence of 2×10^16 cm^-2 and followed by thermal annealing at 673 K for 30 min in vacuum. The internal oxidation is carried out at temperatures ranging from 1073 to 1473 K for 2 h in a dry oxygen atmosphere. The layered structures evolved in the silicon are detected by using the PBA and the thicknesses of their layers and nature are also investigated. It is found that rather high temperatures must be chosen to establish a sufficient flux of oxygen into the cavity layer. On the other hand high temperatures lead to coarsening the cavities and removing the cavity layer finally.     

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.     

Molecular Dynamics Simulations of Helium Behaviour in Titanium Crystals

Molecular dynamics simulations are performed to investigate the behaviour of helium atoms in titanium at a temperature of 30OK. The nucleation and growth of helium bubble has been simulated up to 50 helium atoms. The approach to simulate the bubble growth is to add helium atoms one by one to the bubble and let the system evolve. The titanium cohesion is based on the tight binding scheme derived from the embedded atom method, and the helium-titanium interaction is characterized by fitted potential in the form of a Lennard-Jones function. The pressure in small helium bubbles is approximately calculated. The simulation results show that the pressure will decrease with the increasing bubble size, while increase with the increasing helium atoms. An analytic function about the quantitative relationship of the pressure with the bubble size and number of helium atoms is also fitted.     

Experimental investigation of positron self-trapping near the vapour-liquid critical point of hellium-4

Positron self-trapping in helium near the vapor-liquid critical point is investigated using the positron annihilation lifetime technique. A 13% decrease in the slowing-down time for positrons to reach the self-trapped state is observed at the critical temperature 5.190 K relative to the slowing-down time at 5.200 K.     

He离子注入ZnO中缺陷形成的慢正电子束研究

在ZnO单晶样品中注入了能量为20—100keV、总剂量为4.4×10¹⁵cm^-2的He离子.利用基于慢正电子束的多普勒展宽测量研究了离子注入产生的缺陷.结果表明，He离子注入ZnO产生了双空位或更大的空位团.在400℃以下退火后，He开始填充到这些空位团里面，造成空位团的有效体积减少.经过400℃以上升温退火后，这些空位团的尺寸开始增大，但由于有少量的He仍然占据在空位团内，因此直到800℃这些空位团仍保持稳定.高于800℃退火后，由于He的脱附，留下的空位团 关键词： 慢正电子束 ZnO 离子注入 缺陷     

Defect study on electron irradiated GaAs by means of positron annihilation

Measurements of the positron lifetime and Doppler-broadened annihilation-radiation have been performed in electron-irradiated GaAs. The positron lifetime at the irradiation induced defects was 0.250 ns at 300 K. The defect clustering stage was found to occur at around 520–620 K, and the coarsening and annealing stage is believed to be above 620 K. Similar annealing stages were also observed in GaAs lightly doped with Si (0.2×10¹⁸ cm^–3). Both the lifetime and the S-parameter in the irradiated GaAs were found to decrease with temperature from 300 K to 100 K, suggesting the coexistence of shallow traps in electron irradiated GaAs.     

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.