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.     

Positron studies of hydrogen-defect interactions in proton irradiated molybdenum

Molybdenum single crystals are irradiated at 20 K with 6 MeV protons. The radiation damage and lattice defect annealing is studied by positron lifetime spectroscopy in the temperature range from 15 to 720 K. Loss of vacancies due to recombination with mobile interstitials is observed at 40 K (Stage I) in agreement with resistivity measurements. This is the first time Stage I is observed by positrons below 77 K. The implanted hydrogen decorates the vacancies around 100 K, which is consistent with a hydrogen migration energy in molybdenum:E _M ^H = 0.3–0.4 eV. Clustering of spatially correlated vacancies takes place in a wide temperature region below the usual vacancy clustering stage (Stage III). Stage III is observed at rather low temperatures (400–480 K) due to the very high vacancy concentration. Hydrogen bound to vacancies and vacancy clusters is released above 540 K, which puts an upper limit to the hydrogen binding energy:E _B ^H 1.4 eV. The present work emphasizes the advantage of employing a vacancy sensitive technique to study hydrogen in metals, where its intrinsic solubility is low. In such metals (as molybdenum) both the effective solubility and the effective mobility of hydrogen are strongly influenced by the presence of vacancies.     

Defect study of proton-irradiated liquid-encapsulated Czochralski GaAs using the positron-annihilation technique

The positron lifetime of undoped Liquid-Encapsulated Czochralski (LEC)-GaAs and Si-doped (1.3×10¹⁸ cm^–3) LEC-GaAs was measured before and after irradiation with protons (dose 1×10¹⁵/cm², 15 MeV). In Si-doped GaAs, the decrease of positron lifetime at temperatures between 10 and 300 K are due to the decrease of the positron-diffusion length and the increase of the effective shallow traps such as antisite Ga_As. The annealing stage of the proton-irradiation-induced defects which show the different behavior from that of electron-irradiation-induced defects suggests that proton irradiation creates more complicated defect complexes, containing vacancies rather than isolated vacancy-type defects or simple complexes which have been observed during electron-irradiation processes. Above 700 K, proton-irradiation-induced defects such as vacancy-type defects and simple vacancy complexes are almost annealed out, while Si-induced defects such as Si_Ga-V_Ga complexes cannot be annealed out above 973 K.     

Temperature characteristics of positron trapping at defects in electron-irradiated silicon

Positron-annihilation lifetime and Doppler-broadening measurements are used to investigate defects in silicon irradiated at 373 K with 6 MeV electrons to a dose of 1×l0¹⁹e/cm². In the unirradiated silicon sample (p type) a temperature-independent behaviour of the bulk-lifetime is observed in the temperature interval 110–500 K with a constant value of 220±1 ps. The slight effect observed on the S-parameter evolution is explained taking into account the thermal expansion of the lattice. The lifetime results obtained at 80 K and at 300 K after isochronal annealing as well as the behaviour of the intensity of the second lifetime componentI ₂ during lifetime measurements below the irradiation temperature in the irradiated silicon sample (n type), clearly indicate the temperature dependent characteristics of the positron trapping cross section _t(T) T ⁿ withn= –1.905±0.016. From isochronal annealing results, an annealing stage is observed in which di-vacancies agglomerate into quadri-vacancies. The mean positron lifetime in those quadri-vacancies is 350 ps.A.B.O.S., on leave from University of Kinshasa, Zaïre     

Defects in electron irradiated GaP studied by positron lifetime spectroscopy

Defects induced by electron irradiation were investigated in GaP. The irradiation was performed at 15 K with an incident electron energy of 2 MeV and a fluence of 10¹⁸cm^–2. Annealing experiments were carried out in the temperature range between 100 and 1000 K.Ga and P vacancies were detected after electron irradiation and the different annealing behaviour of the two types of vacancies was observed. The recovery stage between 100 and 400 K was attributed to the annealing of Ga vacancies and the recovery at temperatures above 900 K to the annealing of P vacancies.We also performed Hall measurements to determine the location of the Fermi level in the bandgap during the annealing. Two different ionization levels of the P vacancy were found which can be attributed to the transitions V _P ⁺ /V _P ^o and V _P ^o /V _P ^– .Temperature-dependent measurements were performed to study the effect of shallow positron traps.Paper presented at the 132nd WE-Heraeus-Seminar on Positron Studies of Semiconductor Defects, Halle, Germany, 29 August to 2 September 1994     

Divacancy complexes induced by Cu diffusion in Zn-doped GaAs

Positron annihilation spectroscopy was applied to investigate the nature and thermal behavior of defects induced by Cu diffusion in Zn-doped p-type GaAs crystals. Cu atoms were intentionally introduced in the GaAs lattice through thermally activated diffusion from a thin Cu capping layer at 1100 °C under defined arsenic vapor pressure. During isochronal annealing of the obtained Cu-diffused GaAs in the temperature range of 450?850 K, vacancy clusters were found to form, grow and finally disappear. We found that annealing at 650 K triggers the formation of divacancies, whereas further increasing in the annealing temperature up to 750 K leads to the formation of divacancy-copper complexes. The observations suggest that the formation of these vacancy-like defects in GaAs is related to the out-diffusion of Cu. Two kinds of acceptors are detected with a concentration of about 10¹⁶ ? 10¹⁷ cm^?3, negative ions and arsenic vacancy copper complexes. Transmission electron microscopy showed the presence of voids and Cu precipitates which are not observed by positron measurements. The positron binding energy to shallow traps is estimated using the positron trapping model. Coincidence Doppler broadening spectroscopy showed the presence of Cu in the immediate vicinity of the detected vacancies. Theoretical calculations suggested that the detected defect is V _Ga V _As-2Cu_Ga.     

Positron annihilation at defects in sintered high-T c perovskite superconductors

We report positron lifetime measurements in sintered superconducting YBa₂Cu₃O_7–x and GdBa₂Cu₃O_7–x oxides. It is shown that the thermal behaviour of the positron lifetime spectra strongly depends on the preparation of the ceramics. A lifetime of 190±3 ps is attributed to oxygen deficient regions. Two lifetimes of 251±7 ps and 225 ±5 ps are attributed to a cation vacancy presenting a temperature dependent atomic arrangement. The lifetime transition (251225ps) occurs during decreases in temperature across the resistivity superconducting transition. This lifetime change indicates that the volume of the cation vacancy decreases in the superconducting state.     

Hydrogen indium vacancy complex VInH4 in n-type InP studied by positron-lifetime

Positron-lifetime experiments have been carried out on two undoped n-type liquid encapsulated Czochralski (LEC)-grown InP samples with different stoichiometric compositions in the temperature range 10-300 K. For temperatures below 120 K for P-rich InP and 100 K for In-rich InP, the positron average lifetime began to increase rapidly and then leveled off, which was associated with the charge state change of hydrogen indium vacancy complexes from (V_InH₄)⁺ to (V_InH₄)⁰. This phenomenon was more obvious in P-rich samples that have a higher concentration of V_InH₄. The transformation temperature of approximately 120 K suggests that the complex V_InH₄ is a donor defect and that the ionization energy is about 0.01 eV. The ionization of neutral V_InH₄ accounted for the decrease of the positron average lifetime when the sample was illuminated with a photon energy of 1.32 eV at 70 K. These results provide evidence for hydrogen complex defects in undoped LEC InP.     

Positron annihilation studies on the migration of deformation induced vacancies in stainless steel AISI 316 L

Positron lifetime measurements were carried out at room temperature before and after isochronous annealing of cylindrical, machined fatigue specimens and of round slabs of austenitic stainless steel AISI 316 L deformed in compression. Annealing experiments are evaluated in terms of vacancy migration and sinking to grain boundaries and dislocations. The model assumes spherical grains with a homogeneous initial distribution of vacancies. A vacancy migration enthalpy of H^M _V=(0.9±0.15) eV was found. It is concluded that positron trapping at dislocation lines does not significantly contribute to positron lifetime measurements at room temperature and that single vacancies are the dominating positron traps. Positron annihilation depth profiling on cross-sectional areas prepared from machined specimens using a positron microprobe with 10 μm spatial resolution shows that machining of cylindrical specimens creates vacancies up to 5 mm below the surface. Received: 11 August 2000 / Accepted: 13 November 2000 / Published online: 28 February 2001     

Amorphous hydrogenated silicon studied by positron lifetime spectroscopy

Hydrogenated amorphous silicon (a-Si:H) prepared by dc glow discharge in silane was investigated by positron lifetime measurements at room temperature. The lifetime spectrum shows considerably longer lifetimes than in simultaneously measured Si single crystals. The dominant component with the time constant ₂=402 ps is discussed thoroughly in conjunction with positron trapping at microvoids containing more than 10 to 15 vacancies. Positron trapping at H-saturated dangling bonds cannot be ruled out. The long-lived component with ₃=1800 ps (I ₃=0.06) indicates positronium formation at larger voids.     

A slow positron lifetime study of the annealing behaviour of an amorphous silicon layer grown by MBE

We have studied MBE grown amorphous silicon, which was recrystallized at different temperatures for one hour, with a pulsed positron beam. A positron lifetime of 538±10 ps in the as-grown state is attributed to microvoids containing at least 10 vacancies. An incompletely recrystallized sample annealed at 500°C shows an additional long lifetime from ortho-positronium (o-Ps) pick-off annihilation. The o-Ps component disappears for samples, recrystallized at 700°C and above, and the defect lifetime steadily decreases with higher annealing temperature until a value of 310 ps is reached for the layer annealed at 1200°C. This value is explained by positron trapping at dislocations or small vacancy defects stabilized by dislocations or impurities.Paper presented at the 132nd WE-Heraeus-Seminar on Positron Studies of Semiconductor Defects, Halle, Germany, 29 August to 2 September 1994     

Laser and electrical current induced phase transformation of In<Subscript>2</Subscript>Se<Subscript>3</Subscript> semiconductor thin film on Si(111)

Phase transformation of thin film (∼30 nm)In₂Se₃/Si(111) (amorphous→crystalline) was performed by resistive annealing and the reverse transformation (crystalline→amorphous) was performed by nanosecond laser annealing. As an intrinsic-vacancy, binary chalcogenide semiconductor, In₂Se₃ is of interest for non-volatile phase-change memory. Amorphous In _x Se _y was deposited at room temperature on Si(111) after pre-deposition of a crystalline In₂Se₃ buffer layer (0.64 nm). Upon resistive annealing to 380°C, the film was transformed into a γ-In₂Se₃ single crystal with its {0001} planes parallel to the Si(111) substrate and parallel to Si , as evidenced by scanning tunneling microscopy, low energy electron diffraction, and X-ray diffraction. Laser annealing with 20-ns pulses (0.1 millijoules/pulse, fluence≤50 mJ/cm²) re-amorphized the region exposed to the laser beam, as observed with photoemission electron microscopy (PEEM). The amorphous phase in PEEM appears dark, likely due to abundant defect levels inhibiting electron emission from the amorphous In _x Se _y film.     

Behaviour of vacancies in dilute Fe–Re alloys: a positron annihilation study

Positron annihilation lifetime spectroscopy was used in a room temperature study of the influence of heat treatment on behaviour of vacancies in Fe_0.97Re_0.03 and Fe_0.94Re_0.06 alloys. In this experiment, the vacancies were created during the formation and further mechanical processing of the iron systems under consideration so the lifetime spectra of positrons were collected at least twice. The first samples were taken just after the melting process in an arc furnace, and the second ones were taken for the specimens annealed at 1,270 K and then cold-rolled at room temperature. After that, the spectra were measured for all studied samples after annealing at some temperatures gradually increasing from 300 to 1,270 K. It was found that vacancy-Re pairs are the dominant type of structural defects in alloys just after the melting process. In the case of alloys after a cold rolling process, the dominant type of structural defects is vacancies associated with edge dislocations. Moreover, for cold-rolled samples annealed at 473–573 K, the growth of the vacancy clusters associated with edge dislocations is observed by an increase in the mean positron lifetime. Finally, at temperatures above 573 K, vacancy clusters associated with edge dislocations as well as vacancy-Re pairs become unstable, and freely migrating vacancies sink at grain boundaries.     

Temperature dependence of positron annihilation parameters in neutron irradiated molybdenum

Positron lifetime measurements have been performed for molybdenum samples containing different densities of voids and dislocation loops. The samples consisted of single crystal molybdenum exposed to 2.7×10¹⁸ fast neutrons/cm₂ at 60°C, and subsequently annealed at 650°, 725°, 800°, and 875°C in vacuum (p<10^–7 Torr). After each annealing, where the densities of voids and loops were changed, positron lifetime measurements were performed in the temperature interval [–194°, 285°C]. In two-term fits of the measured spectra the longer lifetime, _e2-460 ps corresponds to an intensityI _e2 increasing with sample temperature. The shorter lifetime _e1 decreases with increasing temperature. A three-state trapping model with and without detrapping is discussed, and appears to be incapable of explaining the observed temperature dependences. A four-state positron trapping model including detrapping is necessary and satisfactory. It describes positron trapping to voids and trapping to dislocation loops, which is followed by a competition between detrapping and positron transition to jogs or other dislocation-bound defects. Mathematical expressions of the four-state trapping model including detrapping are worked out and calculations of the intensityI _e2 are compared with the experimental values ofI _e2. By use of special models for the temperature dependence of trapping rates, numerical values can be determined for the positron-dislocation-binding energy and for specific positron trapping rates.     

The nature of the C-defects in nickel and their rôle in the interpretation of radiation damage in metals

In previous Perturbed-Angular-Correlation (PAC) studies of the - emission of ¹¹¹In probe nuclei in cold-worked or particle-irradiated nickel, it has been found that thermal annealing in the temperature regime of recovery stage III leads to the formation of so-called C-defects (Cubic defects). This is indicated by the occurrence of a new frequency of about 80 Mrad/s, in addition to the frequency (200 Mrad/s) that is due to ¹¹¹In on substitutional sites. Obviously, the C-defects are complexes consisting of ¹¹¹In and the intrinsic point-defect species that migrates freely in recovery stage III. Therefore, they have played an important rôle in the long-standing controversy on whether the recovery-stage-III defects are vacancies (one-interstitial model) or self-interstitials (two-interstitial model). The present paper reports on a novel experimental effort to reveal the nature of the C-defects by combining PAC studies on nickel samples differently pretreated in a systematic way, investigations of the Extended X-ray Absorption Fine Structure (EXAFS) on In-doped nickel, and measurements of the decay rate of ¹¹¹In nuclei in the Electron-Capture-Induced Decay (ECID). On the basis of the results of these experiments it is concluded that the defects trapped by substitutional ¹¹¹In atoms (In_s) in recovery stage III are self-interstitials (I), as expected according to the two-interstitial model. Moreover, there is evidence that the C-defects are In interstitials on tetrahedral sites (In_i) that form exclusively in the vicinity of the specimen surface from In_s – I pairs via the reaction In_s+I In_i.     

Studies on the microstructure of phase transitions in two kinds of liquid crystals by PAT and DSC

The positron lifetime and DSC measerments for EBBA and DOBAMBC have been made with heating and cooling clycles. The experimental results show that a shorter lifetime (₁) is essentially independent of temperature while the longer lifetime (₂) and the intensity (I ₂) change abruptly double or triple with temperature. Consequently, the EBBA has only nematic phases while the DOBAMBC has two liquid-crystalline phases (smectic C* and smectic A) with transition temperatures as follows: for EBBA, solid nematic (304.5 K), nematic isotropic (356.5 K), isotropic nematic (356.5 K), nematic solid (301 K); and for DOBAMBC, solid smectic C* (346 K), smectic C* smectic A (357.5 K), smectic A isotropic (389 K). These critical temperatures are in accordance with the transition temperatures measured by DSC. In addition, the difference in the solid-nematic transition temperature in the heating and cooling cycles was also observed. A discussion about the correlation of the observed changes in lifetime (₂) with the changes in molecular orientational order (S) and dielectric anisotropy () is presented.     

Positron lifetime and 2D-ACAR studies of divacancies in Si

We have measured positron lifetime and Two Dimensional Angular Correlation of Annihilation Radiation (2D-ACAR) distributions of Floating-Zone grown (FZ) Si specimens containing divacancies (V₂) with the definite charge states, V ₂ ⁰ , V ₂ ^–1 or V ₂ ^–2 from room temperature to about 10 K. These charge states are accomplished by an appropriate combination of dopant species, their concentration and irradiation doses of 15 MeV electrons. with reference to the currently accepted ionization level of divacancies. The positron lifetime of the negatively charged divacancy increases with temperature, while that of the neutral divacancy shows little change with temperature. The positron trapping rate, obtained from lifetime and 2D-ACAR measurements, increases markedly with decreasing temperature. This is found not only for the negative divacancies but also for the neutral divacancy. We need a model which explains this temperature dependence. The 2D-ACAR distribution from positrons trapped at divacancies shows nearly the same distribution for the different charge states, which differs considerably from the case of As vacancies in GaAs studied by Ambigapathy et al. We have observed a small but definite anisotropy in the distribution of trapped positrons in V ₂ ^– using a specimen containing oriented divacancies.Paper presented at the 132nd WE-Heraeus-Seminar on Positron Studies of Semiconductor Defects, Halle, Germany, 29 August to 2 September 1994     

Ion irradiation—a technique providing a criterion to distinguish between amorphous and nanocrystalline In1−x Pd x films

In_1–x Pd _x films with 0.2x0.75 have been prepared by vapour quenching at 4.2 K or 77 K, respectively. To test whether amorphous (a-) phases can be obtained in this way, the resistance behavior and the electron diffraction patterns of the as-prepared and annealed films were studied insitu. For films withx=0.25 additional information could be acquired from their superconducting behavior. Combining these results one concludes that a-phases exist for the compositional range 0.2x0.6, which are stable up to crystallization temperaturesT _x within the range 250 KT _x 420 K. Irradiation of the crystallized films at low temperatures (4.2 K or 77 K) with heavy ions (350 keV Ar⁺ or Kr⁺) leads to complete re-amorphization. Forx=0.67 corresponding to InPd₂ a nanocrystalline (n-) phase is obtained by vapour quenching at 77 K as inferred from x-ray diffraction. AtT _x =700 K, thesen-films exhibit a drop of the electrical resistance indicating the beginning of significant grain growth. After recooling, Kr⁺ bombardment at 77 K does not restore the high electrical resistance of the as-quenchedn-film. This result can be used as a criterion when studying quenched films withx=0.625 corresponding to In₃Pd₅. In this case, a resistance drop is found atT _x =600 K, but the diffraction techniques do not allow an uniquevocal distinction between amorphous and nanocrystalline. This becomes possible by low temperature ion irradiation after annealing atT>T _x . The bombardment results in resistance changes, which saturate well-below the value of the as-quenched sample implying nanocrystallinity for the latter. Based on this criterion, a phase-diagram for quenched In_1–x Pd _x is provided with 0x1 containing the newly detecteda- andn-phases.     

Positron annihilation study of alpha-irradiated stainless steel SS 302 and Cobalt

Abstract

Positron lifetime and Doppler broadening measurements have been done to study the α-induced defects in stainless steel SS 302 and polycrystalline cobalt. For stainless steel the samples have been thin and the effect of the presence of helium on defect kinetics has been avoided by allowing the 30 MeV alpha particles to pass through the samples. The presence of impurity (carbon) atoms in steel is found to play an important role in the trapping and detrapping of vacancies in the temperature range 200°C to 450°C. Formation of vacancy-impurity complexes and their dissociation around 500°C have been observed. A steady decrease of the positron parameters has been seen beyond 700°C and they attain those of the reference sample around 1000°C. While annealing alpha irradiated cobalt we find migration of vacancies and rearrangement of dislocation loops below 650 K and then dissolution around 900 K. Helium-vacancy complexes form in the region 600 to 1000 K, leading to the growth of the He-bubble above 1000 K. The trapping model analysis shows strong interaction between He and vacancy clusters in the temperature region 600 to 1000 K.     

Positron annihilation studies of defects in helium-irradiated silicon

Positron annihilation studies have been carried out on Si-n irradiated with He⁺ ions at the V.U.B. cyclotron, to a dose of 4×10¹⁷ He/cm². No temperature dependence on the S-parameter and lifetimes is seen below the irradiation temperature. The positron lifetime associated to the created defects is 290 ps. During the isochronal annealing, this lifetime stays constant up to 700 K. It is attributed to the annihilation of positrons from large vacancy-clusters filled with He atoms. From the isochronal annealing results, only one annealing stage is seen. This annealing stage which extends over a long range of temperature 700–1000 K, is ascribed to the degassing of helium atoms from defects and the growth of vacancy-clusters. The lifetime of positrons in those defects reaches a value of about 530±30 ps at 1000 K, indicating that the vacancy-clusters formed have a mean size of more than 8 vacancies.