Hydrogen and deuterium trapping at nitrogen in tantalum studied by PAC

PAC experiments using¹⁸¹Hf as probe atom were performed in Ta samples containing 1.1 at% of N and loaded with 0.2 at% of H or of 1.6 at% of D. At room temperature only the known frequency due to N is present. Below 100K or 140K, for H and D respectively, the amplitude of this interaction decreases and two new interaction frequencies characterized by V₀=240MHz, η=0.80 and V₀=250 MHz, η=0.40 appear. These frequencies are attributed to H(D) trapped by N in the vicinity of the probe atom¹⁸¹Hf. The disappearance of these interactions at 100K and 140K is interpreted as a release of H (D) from Hf but not from N. From the data the jump rates of H(D) around N in Ta are derived.     

Structure determination of an indium-oxygen-vacancy complex in silver

When bombarding preoxidized silver with α-particles¹¹¹In-oxygen-vacancy complexes are formed. PAC measurements on the most stable complex 6 (ν_q=161 (2) MHz, η=1, δ/ν_q=6(1) %) were performed to determine the structure of this highly asymmetric complex. On the basis of PAC experiments on Ag single crystals and the variation of the oxygen concentration and the measuring temperature a structure model of this complex 6 is proposed.     

The Ag−In intermetallic compound formation from Ag and In electrodeposited layers observed by PAC

The PAC method was applied to study the intermetallic compound formation at Ag−In interfaces. The electrodeposited Ag−In layers of different Ag: In atomic ratios were prepared and isochronal annealing program was performed. For the comparison the bulk Ag₇₅In₂₅ and Ag₆₆In₃₄ specimens were examined. The Ag₂In and AgIn₂ compounds were detected and the quadrupole hyperfine interaction parameters for¹¹¹In in Ag₂In were measured as υ_Q107.9(3) MHz and η=0.48 (2).     

TDPAC characterization of tin oxides using181Ta

In connection with a general study of the evolution of tin-oxygen thin films, we report here on the hyperfine interactions of¹⁸¹Ta substitutionally replacting tin in the isolated phases SnO and SnO₂. For this purpose, pure SnO pressed powder and a thin SnO₂ film were implanted with¹⁸¹Hf. In both cases, unique quadrupole frequencies were found after thermal annealing treatments. The results indicate that the following hyperfine parameters: υ _Q = 740.6(2.1) MHz, η=0.07(2) and υ _Q = 971.5(1.9) MHz, η=0.72(1) characterize¹⁸¹Ta in SnO and SnO₂, respectively.     

Cavity formation at indium impurities in bcc metals

The defect formation in the bcc metals W and Mo above annealing stage III and the influence of rare gases on this process were investigated by means of the perturbed angular correlation technique using¹¹¹In as radioactive probe. In both metals a relatively high electric field gradient (EFG) could be observed at the indium site, characterized by the quadrupole interaction frequencies υ_Q=263 MHz, ν=0 and υ_Q=220 MHz, ν≈0.15 for W and Mo, respectively. The observations are assigned to the growth of threedimensional vacancy clusters at the probe atoms with the indium atoms situated in the inner surface of this cavities, thus experiencing the corresponding surface EFG.     

Temperature dependence of the electric quadrupole interaction at scandium impurities in zirconium and hafnium

The PAC probe⁴⁴Sc was employed to study the magnitude and temperature dependence of the electric quadrupole interaction at the site of the transition metal Sc in the hexagonal host lattices Zr and Hf. In Zr ∼ 100% of the probe atoms were situated on regular lattice sites and a quadrupole interaction frequency of υ_Q=7.8(1)MHz was measured at room temperature. For Hf the fraction of the probe atoms on regular lattice sites was smaller and a damping of the interaction pattern (υ_Q=9.3(5)MHz at 293 K) could not be excluded. The temperature dependence of the electric field gradient in both host lattices was found to be weak.     

Cavities in silicon investigated with the PAC-probe 111In

The perturbed angular correlation technique (PAC) was used to study the creation and development of He-induced cavities. In order to investigate the interaction of Indium atoms with cavities in Silicon the Bonn isotope separator was used to implant overlapping profiles of He (10 keV) and radioactive ¹¹¹In (160 keV) into undoped FZ-silicon. To get insight into the cavity formation mechanism samples were prepared with various He-doses (0.6, 2 and 6× 10¹⁶ ions/cm²). The samples were measured directly after implantation and after different annealing steps (t_hold= 10 min, T = 500–1100oC). Further, different implantation and annealing sequences were used. At higher He doses (2 and 6× 10¹⁶ ions/cm²) we find a large fraction of ¹¹¹In probe atoms subjected to an electric field gradient (EFG) corresponding to a quadrupole interaction frequency (QIF) of ν_Q= 411(6) MHz with η= 0.25(4). The corresponding defect configuration is formed most effectively after He implantation into annealed, ¹¹¹In doped Si. This and the affinity of In to vacancies leads us to the assumption that, similarly to the situation in metals, the Indium atoms act as nucleation centres for vacancy clusters (cavities) and are situated on the inner walls of the cavities. This revised version was published online in August 2006 with corrections to the Cover Date.     

A hydrogen — Vacancy complex at substitutional indium in niobium

The interaction of a In-monovacancy complex in niobium with hydrogen was studied with the PAC-technique between 24 K and 293 K. At 293 K no significant influence of hydrogen on the monovacancy-induced electric field gradient at the In-site was observed. However at a sample temperature ≤ 135 K a new interaction frequency υ_Q3=122(1) MHz, η=O, appears in the spectra, which is assumed to be due to the trapping of hydrogen in a well defined location on the axis between probe nucleus and the monovacancy.     

The electric quadrupole interaction of 111Cd in ZrZn2 and Zn in the samples prepared at 8 GPa

The perturbed angular correlation (PAC) measurements with the ¹¹¹In-¹¹¹Cd nuclear probe embedded into the lattice of the cubic (C15) Laves compound ZrZn₂ showed that ¹¹¹Cd nuclei experienced an axially symmetric electric quadrupole interaction with a frequency ν _Q  = 132.4 MHz at room temperature. The samples were synthesized and doped with the probe at a pressure 8 GPa. The temperature dependence of ν _Q was shown to be linear: ν _Q (T) = 147(1 − 0.033 T) MHz. Since the value of ν _Q is very close to that known for ¹¹¹Cd in the lattice of Zn, we have checked if it could be assigned to residual Zn metal in the sample. For the Zn sample melted and doped with ¹¹¹In at 8 GPa we have obtained ν _Q  = 117.3 MHz at 300 K and 127 MHz at 80 K – both values considerably lower than that for ¹¹¹In doped Zn samples prepared at an ambient pressure. These data, and the fact that ν _Q (T) in Zn is known to follow the T ^3/2 law, allow to attribute the ν _Q value quoted above to ¹¹¹Cd nuclei at the substitutional sites with tetrahedral symmetry in the Zn sublattice of ZrZn₂.     

Fluctuating Electric Field Gradients at 111Cd in Ice

¹¹¹Cd–PAC measurements have been made using the high specific activity of ¹¹¹In in the methanol–water mixtures of various concentrations at the room temperature. These experiments revealed that the perturbation factors 〈A ₂ G ₂〉 (integrated over two mean lives τ_N) do not follow the dependence of the macroscopic viscosity η. The observed dynamic character of the PAC spectra in ice is explained by the mobility of orientational and ionic defects. The activation energy for the diffusion process was determined to be E _a =0.35(1) eV. This revised version was published online in September 2006 with corrections to the Cover Date.     

Mössbauer and XRD Comparative Study of Host Rock and Iron Rich Mineral Samples from Paz del Rio Iron Ore Mineral Mine in Colombia

The local environment of implanted ¹¹¹Ag (t _1/2 = 7.45 d) in single-crystalline [0001] ZnO was evaluated by means of the perturbed angular correlation (PAC) technique. Following the 60 keV low dose (1 × 10¹³ cm⁻²) ¹¹¹Ag implantation, the PAC measurements were performed for the as-implanted state and following 30 min air annealing steps, at temperatures ranging from 200 to 1050°C. The results revealed that 42% of the probes are located at defect-free S_Zn sites (ν _Q ∼ 32 MHz, η = 0) in the as-implanted state and that this fraction did not significantly change with annealing. Moreover, a progressive lattice recovery in the near vicinity of the probes was observed. Different EFGs assigned to point defects were furthermore measured and a general modification of their parameters occurred after 600°C. The 900°C annealing induced the loss of 30% of the ¹¹¹Ag atoms, 7% of which were located in regions of high defects concentration.     

Nuclear quadrupole interactions at 187W(β-) 187Re in ZrW2O8

In ZrW₂O₈, a material with negative thermal expansion, two nuclear quadrupole interactions at ¹⁸⁷W(β^-) ¹⁸⁷Re with equal populations were determined by time differential perturbed angular correlation to be (at 295 K): ν_{\mathrm{Q} 1} = 336(1) MHz, η₁ = 0 and ν_Q2 = 1391(2) MHz, η₂ = 0.053(4). The nuclear quadrupole interactions are assigned to two crystallographically distinct tungsten sites. These results are the bases for further TDPAC studies of the negative thermal expansion on a microscopic scale. This revised version was published online in August 2006 with corrections to the Cover Date.     

Indium metal nanoclusters studied by PAC

The technique of perturbed angular correlations of gamma rays (PAC) is applied for the first time to study the structure of small metal clusters. Metal clusters containing¹¹¹In probe atoms with 50 nm radii were synthesized by dissolving InCl₃ containing¹¹¹In in hexane using a surfactant, thereby creating an inverse micellar solution. The salt was then reduced to metal form by addition of NaBH₄. 100% conversion efficiency of In salt to metal clusters was achieved. PAC measurements at 293 K on the¹¹¹Cd daughter nuclide exhibited a nuclear quadrupole interaction with coupling frequency ₀=16.0(5) Mrad/s and a small asymmetry parameter, =0.20(4). The frequency is as observed for bulk In crystals, but a non-zero value of has not been previously reported. Lack of inhomogeneous signal broadening and the faceted shape of some nanoclusters suggest high crystal perfection.     

Intrinsic point defects in niobium: Trapping at100Pd and111In impurities observed by PAC

Radiation-induced lattice defects in high-purity niobium have been investigated in the temperature range of 30K to 540 K by means of - perturbed angular correlation (PAC) measurements using the radioactive probes¹⁰⁰Pd/¹⁰⁰Rh and¹¹¹In/¹¹¹Cd. Both probes were produced within the niobium samples by means of heavy-ion nuclear reactions. At the Pd impurities trapping of defects occurred during heavy-ion irradiation at about 30 K in two defined configurations: defect 1(Pd) withv _Q1=e ² qQ/h=42(±2) MHz, ₁=0 and defect 2 (Pd) withv _Q2=(±2) MHz, ₂=1. Two defects were observed at the In impurities in annealing stage III (around 250 K) after heavy-ion as well as electron irradiations: defect 1(In) withv _Q1=87(±1) MHz, ₁=0 and defect 2(In) withv _Q2=105(±2) MHz, ₂=0.65(±0.02). A third defect (defect 3(In):v _Q3=177(±2) MHz, ₃0.2) appeared above 260 K after heavy-ion irradiation only. The data are interpreted in terms of interstitial trapping at the Pd impurities and vacancy trapping at the In impurities. Information on the microscopic structure of defect 1(In) and 2(In) is obtained from a PAC-single-crystal experiment. For defect 1(In) axial 111-symmetry is found, which leads us to identify this defect with a monovacancy as nearest neighbor with respect to the In probe. Defect 2(In) is the trapped divacancy for which an orientation is found that is consistent with both vacancies being nearest neighbor to the probe but second nearest neighbors to each other.     

Electric-Field Gradients at Group-III Sites on GaAs and InAs (111)B Surfaces

We report a comparison of electric-field gradients (EFGs) measured at the group-III sites on epitaxially-grown surfaces of 2×2-reconstructed GaAs and InAs crystals. For this purpose, we used ¹¹¹In→¹¹¹Cd perturbed-angular-correlation (PAC) spectroscopy. Sharp spectral lines characterize the perturbation functions corresponding to both surfaces. On GaAs surface, we observe only one well-defined nuclear electric-quadrupole interaction (NQI); and on the InAs surface, we observe a primary and a secondary NQI. Very similar but experimentally-distinguishable values of the EFG-parameters characterize the primary interactions corresponding to the GaAs and InAs surfaces. Specifically, for the GaAs and InAs surfaces, ω _Q =28.0±0.2 Mrad s⁻¹ and η=0.43±0.02 and ω _Q =28.8±0.2 Mrad s⁻¹ and η=0.39±0.02, and the angles between EFG z-axis and the (111) direction are 65°±3° and β=53°±3°, respectively. These unexpected results indicate that the so-called lattice contribution to the EFG is not significant. Moreover, for the primary NQIs on both surfaces, the similar parameter values demonstrate that chemical differences between the ¹¹¹In probe and the indigenous Ga surface atoms cause no large quantitative effects. This information indicates that impurity probes and PAC spectroscopy can be used effectively to investigate III–V surfaces. This revised version was published online in September 2006 with corrections to the Cover Date.     

TDPAC studies of Hf doped YBCO

Time differential perturbed angular correlation measurements of the 133–482 keVγ-γ cascade of¹⁸¹Ta in Hf-doped YBa₂Cu₃O_7−x are presented. The¹⁸¹Hf precurser nuclei are incorporated into the sample by thermal neutron irradiation. Two quadrupole interaction frequencies are observed in the as-irradiated sample:v _Q1=161±10 MHz with intensityf ₁=75%, asymmetry parameterη ₁=0.32 and damping parameter Λ₁=0.42, andv _Q2=1108±40 MHz withf ₂=25%,η ₂=0.62, and Λ₂=0.60. On annealing the sample in air at various temperaturesT _a and quenching to room temperature,f ₁ remained nearly constant forT _a<600°C andv _Q1 for all annealing temperatures indicating that these are insensitive to oxygen stoichiometry. This frequency is interpreted to be due to¹⁸¹Hf substitutingY sites. BeyondT _a=600°C,f ₁ increased and reached a constant value of 90% forT _a=800°C. The value ofv _Q2 showed a slight variation between 1086 and 1160 MHz, whilef ₂ remained nearly constant at 25% forT _a<600°C. This component is identified to be due to¹⁸¹Hf substituting Cu 1 sites in the Cu-O chains of YBCO. Above 600°Cv _Q2 decreased and reached a value of 808 MHz beyond 750°C.     

Probing grain boundaries in As-doped polycrystalline silicon

Using ¹¹¹In–¹¹¹Cd perturbed angular correlations, we investigated the behaviour of In in heavily As-doped polycrystalline silicon. The nuclear In tracers were either introduced by means of grain boundary (GB) diffusion or ion implantation. We find, that the in-diffused In tracers exclusively probe GBs which give rise to a broad distribution of static quadrupole frequencies. The implanted tracers exclusively probe Si bulk material, where they encounter As-dopants during thermal annealing and form the well-known In–As complexes #1 and #2, and the previously unknown complex #4 (eQV_zz=117 MHz, η=0) which involves three As atoms on nearest neighbor sites with respect to the probe. The implications of the present experiment on acceptor doping and GB probing are discussed. This revised version was published online in August 2006 with corrections to the Cover Date.     

PAC-study of defects in n-type germanium

Using perturbed angular correlations of γ rays the behaviour of Frenkel defects in n-type germanium is studied.¹¹¹In/¹¹¹Cd probes either serve as primary knock-on atoms in the production of Frenkel defects by neutrino recoil or as trapping agents for defects produced by electron irradiation. The neutrino recoil process leads to a defect which is characterized by vQ=e²qQ/h=42(2) MHz (η=0.6), while a defect with vQ=423(1) MHz (η=0) is observed after electron irradiation and thermal annealing.     

Hyperfine interaction of111Cd in antiferromagnetic cobalt oxide

The temperature dependence of the hyperfine field of substitutional¹¹¹Cd in antiferromagnetic CoO has been measured by means of the perturbed angular correlation technique. The Larmor frequency ω_L is found to obey a power law ω_L(t=ω₀ t ^β) up tot _max=0.4 wheret=1−T/T _N is the reduced temperature withT _N=291.2(3) K and β=0.393 (5) the critical exponent. The results are discussed and compared with PAC experiments on¹¹¹Cd in NiO and Ni and with results obtained by other methods.