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.
Ferroelectric lithium niobate crystals offer a great potential for applications in modern optics. To provide powerful optical components, tailoring of key material parameters, especially of the refractive index n and the ferroelectric domain landscape, is required. Irradiation of lithium niobate crystals with accelerated ions causes strong structured modifications in the material. The effects induced by low-mass, high-energy ions (such as 3He with 41 MeV, which are not implanted, but transmit through the entire crystal volume) are reviewed. Irradiation yields large changes of the refractive index Δn, improved domain engineering capability within the material along the ion track, and waveguiding structures. The periodic modification of Δn as well as the formation of periodically poled lithium niobate (PPLN) (supported by radiation damage) is described. Two-step knock-on displacement processes, 3He→Nb and 3He→O causing thermal spikes, are identified as origin for the material modifications.
Positron annihilation spectroscopy was performed to study the microstructure of peak aged Al-Zn-Mg-Cu alloy Applying artificial ageing at different temperatures, the solute content around vacancies is found to be increased compared to as quenched state The similarity of vacancy surroundings of all artificially aged states, except for over-aged ones, suggests that peak strength is caused not only by eta' precipitates but also by GPII zones Moreover, eta' precipitates produced by artificial aging at 403 K are apparently coherent with the Al matrix (C) 2010 Acta Materialia Inc Published by Elsevier Ltd All rights reserved
A lot of light aluminium alloys achieve their favourable mechanical properties, especially their high strength, due to precipitation of alloying elements. This class of age hardenable Al alloys includes technologically important systems such as e.g. Al-Mg-Si or Al-Cu. During ageing different precipitates are formed according to a specific precipitation sequence, which is always directed onto the corresponding intermetallic equilibrium phase. Probing the defect state of individual precipitates requires high spatial resolution as well as high chemical sensitivity. Both can be achieved using the finely focused positron beam provided by the Bonn Positron Microprobe (BPM) [1] in combination with the High Momentum Analysis (HMA) [2]. Employing the BPM, structures in the micron range can be probed by means of the spectroscopy of the Doppler broadening of annihilation radiation (DBAR). On the basis of these prerequisites single precipitates of intermetallic phases in Al-Mg-Si and Al-Cu, i.e. Mg2Si and Al2Cu, were probed. A detailed interpretation of these measurements necessarily relies on theoretical calculations of the DBAR of possible annihilation sites. These were performed employing the DOPPLER program. However, previous to the DBAR calculation the structures, which partly contain vacancies, were relaxed using the ab-initio code SIESTA, i.e. the atomic positions in presence of a vacancy were recalculated.
Radiation damage in magnesium-doped lithium niobate crystals, created by low-mass, high-energy ions which have transmitted the entire crystal thickness, leads to an enhanced electrical dark conductivity as well as an enhanced photoconductivity. Experimental results on the electrical properties after ion exposure are given, and an asymmetric dependence of the conductivity as well as refractive index changes on the irradiation geometry with respect to the ferroelectric axis is revealed.
The influence of microalloying additions of Au to the binary Al–Cu system is investigated utilizing hardness measurements, positron annihilation spectroscopy and X-ray absorption spectroscopy. No room temperature ageing could be observed in the case of the ternary Al–Cu–Au alloy. Instead, quenched-in vacancies were trapped by Au atoms and thus could not catalyse the decomposition of the alloy. However, artificial ageing dissolves the complexes of Au and vacancies. A comparison between experimental and calculated absorption spectra shows that Au atoms did not agglomerate significantly during either natural or artificial ageing.
The concentration of lattice defects in plastically,deformed metals can be measured by positron annihilation spectroscopy (PAS) with an outstanding sensitivity. The positron acts as a highly mobile atomic probe sensitive to all defects forming an open volume in the lattice. Using a positron microbeam, like the Bonn positron microprobe (BPM), the lateral distribution of these defects in the sub-surface layer can be mapped with a resolution down to one micrometer. In this work the changes in the defect concentration were determined during tension tests on the aluminium alloys AA2024, AA6013 and AA6082. The results show that these changes depend on the configuration and the heat treatment of the alloys. Moreover, alternating load fatigue tests were performed on AA6082. The defect distribution was measured laterally resolved employing the BPM in several early stages of fatigue. Using those results the number of cycles to fatigue failure was extrapolated. The trueness of the prediction was tested by further fatiguing the sample until failure occurs. (C) 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Nb K-edge x-ray absorption fine structure spectra from a single lithium niobate (LN) crystal irradiated with high-energy 3He ions of 41 MeV and from unexposed crystal as the reference material are compared. The differences in the x-ray absorption near edge structure (XANES) spectra are interpreted by simulating Nb K-edge XANES spectra with the FEFF8.2 code. It is found that displacements of Nb and Li atoms, as well as Li and O vacancies, are likely to cause structural disorder leading to change in the refractive index of LN and to diminished birefringence. This finding is in agreement with previous results obtained from SRIM-2003 simulations and transmission electron microscopy measurements.
Congruently melting undoped lithium niobate crystals are irradiated with 20 MeV(3) He ions which penetrate the entire crystal volume. Radiation damage effects are directly visualized by transmission electron microscopy (TEM) where damage zones with diameters of 4 nm give rise to circular Fresnel fringe contrasts. These regions of modified material, appearing circular in cross-section, are interpreted as damage cascades inflicted by fast Nb and O atoms displaced in knock-on collisions with primary (3)He ions. This two-step displacement process results in local density changes manifested by the contrast behaviour of Fresnel fringes observed in TEM images.
Irradiation of 5% magnesium-doped lithium niobate crystals (LiNbO 3 :Mg) with high-energy, low-mass 3 He ions, which are transmitted through the crystal, changes the domain reversal properties of the material. This enables easier domain engineering compared to non-irradiated material and assists the formation of small-sized periodically poled domains in LiNbO 3 :Mg. Periodic domain structures exhibiting a width of ≈520 nm are obtained in radiation-damaged sections of the crystals. The ferroelectric poling behavior between irradiated and non-treated material is compared.
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)
Irradiation of optical damage resistant, magnesium doped lithium niobate crystals with fast, high-energy He2+3 ions changes important material properties. In the interaction region, where the ions transmit through the material, the ferroelectric coercive field EC is diminished from 6.0kVmm−1 down to 5.0–5.4kVmm−1 after transmission of 41MeV He2+3 particles. This enables easier domain reversal in irradiated crystals compared to untreated material. Besides, large changes of the refractive index of the crystals on the order of 6×10−3 are induced by the treatment. Moderate annealing treatments do not diminish Δn, but refresh the coercive field.
For the neutrino mass determination experiment KATRIN, the long-term stability of the spectrometer voltage is of crucial importance. Therefore, it is planned to control the voltage continuously in a smaller spectrometer, which monitors the position of the conversion electron line emitted in the 32 keV transition in the decay of (83m)Kr. Due to the short half-life of (83m)Kr (t(1/2)=1.83h), it has to be supplied by a long-lived (83m)Kr((83)Rb) generator (t(1/2)=86d). Here, a hitherto unexploited method for the efficient production of (83)Rb and its suitability for its application in the KATRIN monitor spectrometer is described.
We propose X-ray absorption (XAS) measurements as a novel approach to determine the atomic structure of pre-Guinier-Preston zones. These nano-clusters are formed during very early stages of aging AlCu alloys, immediately after solution heat treatment and quenching. X-ray absorption near-edge structure (XANES) spectra were taken from technical aluminum alloys at the copper K edge, revealing the local atomic environment of copper. The spectra of - after solution heat treatment - freshly quenched and of artificially aged alloys differ significantly from each other. We compare the measured XANES spectra with those calculated by the FEFF-8 code. We show the importance of employing realistic, i.e. relaxed, atomic coordinates around the scattering atom type from ab-initio calculations with SIESTA. Atomic structure of a pre-GPZ from SIESTA: a small disk of five Cu atoms (red) on a {100} plane in fcc Al (blue). Note that Al atoms in direct neighborhood of copper relax towards the small Cu disk. (online colour at: www.pss-rapid.com) (c) 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Several samples of the common ferritic tool steel AISI 1045 were fatigued in cyclic load tests. The local distribution of the Von-Mieses stress sigma(VM) was simulated using the finite elements method (FEM). In the regions of interest, where sigma(VM) reaches maximum values, the defect distribution was measured spatially resolved by Doppler-spectroscopy (DBAR) employing the Bonn Positron Microprobe (BPM). The lateral distribution of the S-parameter, which could be described by a simple model derived from linear fracture mechanics, corresponds well with the simulated Von-Mieses stress. (c) 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
In this letter, the authors elaborate a detailed study of ion-implanted GaAs terahertz photomixers. The authors implanted several GaAs samples with oxygen and nitrogen ions with energies between 2 and 3MeV and doses ranging from 2×1011to3×1013cm−2. The samples were processed by patterning metal-semiconductor-metal structures on the feed point of self-complementary log-periodic spiral broadband antennas. From dc measurements and analysis of frequency roll-off in the 100GHz–1THz range under variable bias conditions, the authors studied systematically the carrier trapping time, terahertz power, and photocurrent dependence on applied voltage and frequency for the different samples.
We present a novel way for recording a rid mathematically analyzing the Doppler-broadening of the 511 keV annihilation line to obtain the momentum distribution of the annihilating electron-positron pair. A necessary precondition is employing either background free positron or e.g. a Ge-68-source, instead of the widely used positron emitter Na-22. The Ge-68-source emits positrons with in end-point energy of about 1.9 MeV, while the contribution of gamma quanta having higher energies than the annihilation radiation at 511 keV is negligible low. Compared to Na-22, this results ill a significant lower background ill the photo peak. Employing such a (68)Gesource allows an analysis of the high-momentum part of the annihilation radiation. However, this part contains valuable chemical information about the annihilation site of the positron, originating from high momentum electrons. Providing all adequate mathematical analysis in determining the remaining background and its subsequent subtraction, we are able to obtain the contribution of these high electron momenta to the annihilation peak using only a single Ge-detector. After background subtraction, the same information contained in the momentum range tip to 35 x 10(-3) m(0)c can be extracted by analyzing spectra from metals and semiconductors as if measured employing a coincidence setup with two Ge-detectors. With the method presented here it is possible to obtain the whole information of a positron annihilation Doppler spectrum employing just a single Ge-detector. (c) 2006 Elsevier B.V. All rights reserved.
Irradiation of lithium-niobate crystals (LiNbO3) with fast, high-energy 3He ions changes the refractive index in the interaction region where the ions speed through the material. Thus an inhomogeneous flux density profile can be used for a tailored modification of the optical properties of LiNbO3 crystals, without employing ion implantation. A new method to fabricate embedded, polarization sensitive channel waveguides in LiNbO3 utilizing accelerated 3He ions with an energy of 40 MeV is demonstrated.
Proton pulse NMR, established as a versatile method in Solid State Physics, Chemistry, Biology and Medical Science, requires on the order of 1018 nuclei to detect an electromagnetic signal in a free induction decay (FID). The main cause for this small sensitivity is the low polarisation in the order of a few ppm due to the Boltzmann distribution in the magnetic field. Thus, NMR experiments on hydrogen are limited to metals with extremely high hydrogen solubility like Pd near room temperature. Using a polarised proton beam, a NMR signal is possible with as few as 1013 implanted nuclei. For the first time spin–spin and spin–lattice relaxation times were measured in Au and W with this technique at the Bonn cyclotron.