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.     

A positron remoderator for the high intensity positron source NEPOMUC

A remoderator for the high intensity positron source NEPOMUC was developed and installed at the beam facility. A beam of remoderated positrons could be produced with different energies and a diameter of less than 2 mm was obtained. The efficiency of the remoderation setup was determined to be 5%. Due to the brilliance of the remoderated beam, the measurements at the coincidence Doppler broadening spectrometer (CDBS) and at the positron annihilation induced Auger electron spectrometer (PAES) could be improved. The setup and functionality of the remoderation device is presented as well as the first measurements at the remoderator, CDBS and PAES.     

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).     

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.     

A technique for positron spectroscopy of monovacancies formed by low-temperature ion implantation of silicon

A system for positron beam-based Doppler broadening spectroscopy of the formation and evolution of monovacancy defects in silicon is described. The apparatus allows in situ ion implantation at low temperatures (∼50 K) followed by positron beam assay. First measurements for 6 keV He implantation, at post-implant temperatures between 60 and 300 K are presented. Benefits and drawbacks of this system are discussed.     

A study of defects in deformed FeSi alloys using positron annihilation techniques

Steels with high amounts of silicon are used in electrical applications due to their low magnetostriction, high electrical resistivity and reduced energy losses, but they exhibit poor formability. The slow positron beam of Gent is used to investigate defects in different deformed FeSi alloys. It was found that the concentration of defects for the alloys deformed at high temperatures are different from the ones related to the alloys deformed at room temperature. These results are correlated to the results of positron annihilation lifetime spectroscopy (PALS).     

Vacancy defects induced in sintered polished UO2 disks by helium implantation

Vacancy defects have been investigated in sintered polished and annealed uranium oxide disks. Slow positron beam coupled with Doppler broadening spectrometer was used to probe the track region of 1 MeV ³He ions implanted in uranium dioxide (UO₂) disks. The low and high momentum annihilation fractions, S and W, respectively, were measured in the first micrometer near surface region of the disks as a function of positron energy. The S and W values indicate that the 1 MeV He ions induce vacancy defects in the track region of their range. The vacancy defect depth distribution is heterogeneous. The positron trapping at these vacancy defects increases with the depth and with the implantation fluence indicating an increase of the vacancy defect concentration. The nature of the induced vacancy defects does not change with the fluence.     

GaN-a new material for positron moderation

GaN with its wide bandgap might be of interest as a positron moderation material in much the same way as SiC is. To investigate this, positron beam experiments have been performed to establish the diffusion behaviour and surface branching of positrons implanted with energies varying from 0 to 25 keV into an epitaxially grown layer of semi-insulating GaN on a sapphire substrate. The measured diffusion length of the positrons amounted to 19.3 ± 1.4 nm. The surface branching ratios were as follows: 48% positron emission, 12% positronium formation and 40% trapping at the surface. The positron workfunction was shown to be negative with a value of 2.4 ± 0.3 eV. The materials feasibility for positron moderation and its possible use in field assisted moderation is discussed.     

Performance of the Beijing pulsed variable-energy positron beam

In order to study the depth-dependent characteristics of open-volume defects in thin surface layers, the variable-energy positron lifetime spectroscopy (VEPLS) has been enabled by pulsing a continuous positron beam. The buncher is a quarter-wave coaxial resonator and the RF-signal is fed in by a coupling loop with a frequency of 149.89 MHz and the reflection factor of 0.05 measured by a Network Analyzer. Three synchronic signals with their phases and amplitudes adjusted independently are supplied for start signal of the positron lifetime measurement and the power signal by an electronic system. The stop signal is derived from a detector, a BaF₂ scintillator coupled to a photomultiplier-tube (Hamamatsu). The time resolution of 295 ps (FWHM) was achieved for a Kapton film and a Ti sample at positron energies in the range between 1 keV and 30 keV.     

On the defect pattern evolution in sapphire irradiated by swift ions in a broad fluence range

Sapphire samples, irradiated with swift Kr (245 MeV) ions at room temperature in a broad fluence range, were investigated using a continuous and a pulsed positron beam to study the defect structure created by the passage of the ions in depths of a few micrometers. At small doses, monovacancies were identified as dominant defects and positron trapping centres. These monovacancies are assumed to be highly concentrated inside a cylindrical volume around the ion path with an estimated radius of ∼1.5 nm. For higher doses a second type of trapping centre emerges. This second class of structural imperfection was associated with the overlap of the individual ion tracks leading to the formation of larger vacancy clusters or voids.     

Performance of a slow positron beam using a hybrid lens design

The University of Hong Kong positron beam employs conventional magnetic field transport to the target, but has a special hybrid lens design around the positron moderator that allows the beam to be focused to millimeter spot sizes at the target. The good focusing capabilities of the beam are made possible by extracting work-function positrons from the moderator in a magnetic field free region using a conventional Soa lens thus minimizing beam canonical angular momentum. An Einzel lens is used to focus the positrons into the magnetic funnel at the end of transportation magnetic field while at the same time bringing up the beam energy to the intermediate value of 7.5 keV. The beam is E × B filtered at this intermediate energy. The final beam energy is obtained by floating the Soa-Einzel system, E × B filter and flight tube, and accelerating the positrons just before the target. External beam steering saddle coils fine tune the position, and the magnetic field around the target chamber is adjusted so as to keep one of the beam foci always on the target. The system is fully computer controlled. Variable energy-Doppler broadened annihilation radiation (VEDBAR) data for a GaN sample are shown which demonstrate the performance of the positron beam system.     

Evidence of formation of tetravacancies in uniformly oxygen irradiated n-type silicon

High purity n-type silicon single crystal with resistivity in the order of 4000 Ω cm has been irradiated with high-energy oxygen ions at room temperature up to a fluence of 5E15 ions/cm². The energy of the beam was varied from 3 to 140 MeV using a rotating degrader to achieve a depthwise near-uniform implantation profile. Radiation induced defects and their dynamics have been studied using positron annihilation spectroscopy along with isochronal annealing up to 700 °C in steps of 50 °C for 30 min. After annealing the sample at 200 °C for 30 min, formation of silicon tetravacancies has been noticed. The formation of the tetravacancies was found to be due to agglomeration of divacancies present in the irradiated sample. An experimentally obtained positron lifetime value of 338±10 ps has been reported for silicon tetravacancies, which has a very close agreement with the value obtained from recent theoretical calculations. The tetravacancies were found to dissociate into trivacancy clusters upon further annealing. The trivacancies thus obtained were observed to agglomerate beyond 400 °C to form larger defect clusters. Finally, all the defects were found to anneal out after annealing the sample at 650 °C.     

Planned positron experiments at FRM-II

The new research reactor FRM-II near Munich has a strong positron source, which delivers an intense, nearly monoenergetic positron beam. Our positron systems, the pulsed low energy positron source (PLEPS) and the scanning positron microscope (SPM) will be operated at this beam. Some aspects of matching these systems to the new positron source will be discussed.Considerable improvements are expected, e.g. more than 10⁵ s⁻¹ recorded events at PLEPS and sub-micrometre resolution at SPM. They will enable investigations in so far inaccessible problems like the evaluation of annihilation characteristics and trapping constants of individual defects or studies of fast dynamical processes. In applied materials science complex defect structures will be studied which demand a resolution into many differing lifetimes, e.g. fractured specimens, wear, corrosion, etc. Also large series of measurements at small systematic modifications are planned. There is also the opportunity to analyse in addition the chemical microstructure of the specimens by means of a hydrogen microprobe and other ion beam techniques available close to FRM-II at the Technical University of Munich.     

Status of an R&D project of a positron gun at “Horia Hulubei” NIPNE Bucharest

A new positron gun (PG) will enable high sensitivity measurements in applications of positron annihilation spectroscopy in Romania. Some data concerning the design of a modular system for focussing, transport and acceleration of mono-energetic positrons in the range 0.8-50 keV have been obtained and experimenting on moderators and CDBS was performed. We present a short overview of the present status of the project and preliminary results from Coincidence Doppler Broadening Spectroscopy with a ²²NaCl source, on Al samples. The entire positron gun system will be designed as a high-vacuum dedicated extension operating with two options: a 50 mCi ²²NaCl source and in-line with the NIPNE cyclotron or a new intense compact cyclotron.     

Defect studies of hydrogen-loaded nanocrystalline Gd films

The present work reports on microstructure investigations of hydrogen-loaded nanocrystalline Gd films by means of slow positron implantation spectroscopy combined with in situ synchrotron radiation X-ray diffraction. It is found that the virgin films contain a high density of vacancy-like open volume defects at grain boundaries which trap positrons. These defects represent trapping sites also for hydrogen. With increasing hydrogen concentration the transformation from the α- into the β-phase (GdH₂) takes place in the film. Accumulation of hydrogen at grain boundaries causes a decrease of positron localization at defects. The transformation into the β-phase is completed at x_H ≈ 1.6 H/Gd. Contrary to bulk Gd specimens, the γ-phase (GdH₃) is not formed in the nanocrystalline Gd films.     

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.     

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.     

First positron experiments at NEPOMUC

The in-pile positron source NEutron induced POsitron source MUniCh (NEPOMUC) of the new Munich research reactor FRM-II is now operated at the nominal reactor power of 20 MW. Recently, intensity and positron beam profile measurements were performed at 30 eV and 1 keV, respectively. For this purpose, NaI-scintillators detect the 511 keV γ-radiation of positrons that annihilate at a removable target in the beam line. The beam profile is determined with a micro-channel plate detector and a CCD-camera. In the present arrangement of NEPOMUC's instrumentation the positron beam is connected to a coincident Doppler broadening (CDB) facility and to a positron induced Auger electron spectroscopy (PAES) analysis chamber. First experiments were carried out in order to show the performance of these new spectrometers. An overview of the positron beam facility is given and first experimental results of PAES are presented.     

Al-4%Ag合金中Ag原子偏析的低温正电子湮没参数研究

分别研究了823 K淬火处理和20%形变量的Al-4%Ag低温下Ag析出物对正电子的捕获行为的变化。采用正电子湮没寿命谱(PALS)技术和符合多普勒展宽能谱(CDBS)在温度范围10~293 K内对其进行表征。多普勒展宽能谱结果表明2种样品中均存在Ag析出物。正电子寿命谱的解谱结果中的各组分给出了Ag析出物随测量温度的变化规律。在170 ~273 K之间,正电子湮没行为具有较强的温度依赖性。但对于两个具有不同类型缺陷的样品,在低于170 K时观察到样品中Ag析出物捕获正电子能力出现了差异。随着测量温度的降低,淬火样品中的Ag析出物的正电子寿命和强度基本不变。在低于170 K的测量中,形变样品中的Ag析出物对正电子的捕获能力仍旧存在着较强的温度依赖性,但是变化幅度在逐渐减弱。当测量温度提升到室温(273~293 K),越来越多的正电子从Ag析出物中逃逸,逐渐回到自由状态或被其他深陷阱所捕获,失去了对温度的依赖性。     

Evolution of pores in mesoporous silica films: Porogen loading effect

Mesoporous silica films were synthesized via a sol-gel process under an acidic condition. Various amounts of triblock copolymer F38 were loaded to precursor sols as the pore generator. The evolution of the pores generated by porogen decomposition was investigated as a function of F38 loading by positron annihilation gamma-ray energy spectroscopy and positron annihilation lifetime spectroscopy based on slow positron beams. The threshold of pore percolation is found to be around 10 wt% of F38 loading by positron annihilation gamma-ray energy spectroscopy. Positron annihilation lifetime spectroscopy in the films show that the pore size increases from 1 nm to 3 nm with increasing F38 loading from 5 wt% to 30 wt%.