Positron annihilation studies of defects in 3CSiC hot-implanted with nitrogen and aluminum ions

2 ⁺ and Al⁺ at temperatures from room temperature (RT) to 1200 °C at doses of 10¹³ and 10¹⁵/cm². It is found from Doppler broadening spectra of annihilation gamma-rays obtained by varying the incident positron energy that hot-implantation gives rise to clustering of vacancies, whereas it suppresses amorphization and diminishes the thickness of damaged layers. The average size of such clusters increases with increasing implantation dose and temperature. Vacancy clustering by hot-implantation can be interpreted by the combination of vacancies during implantation. Vacancy type defects in the low-dose (10¹³/cm²) implanted samples are found to be removed by annealing at 1400 °C, whereas large vacancy clusters still remain after 1400 °C annealing in the high-dose (1 0¹⁵/cm²) implanted samples. It is also derived from the depth profile of positron diffusion length that positron scattering centers are produced after annealing at 1400 °C in all implanted samples. Received: 7 March 1997/Accepted: 6 May 1997     

Field emission studies of oxygen on silver tips

Clean [111] oriented silver field emitting tips have been exposed to oxygen at 10^?3 Torr for 1 min at temperatures ranging from ? 170 to 200°C. From 50 to 200°C, an adsorption structure is formed that is stable in oxygen. The structure is characterized by intensely emitting regions on either side of enlarged {110}, {210} and {310} faces and a dark region in the (111)-{100} zone line directions. For adsorption from ? 170 to 200°C, the structure of the patterns depends distinctly on the adsorption temperature because the coverages are different and adsorption is activated. Oxygen adsorption at 10^?3 Torr for 1 min at 0°C causes an increase in the average work function of 1.15 eV. At 0°C, silver was exposed increasingly at 10^?6 Torr until 6100 L was reached. The work function increased progressively by 0.61 eV for this exposure. The {111}, {100}, {311}, {211} and {533} faces are attacked first. Then, the {110} faces are attacked followed by the {210} {310} and {320}. Heating of the adsorption layer formed at 0°C produced no changes in pattern and work function up to 100°C. Between 100 and 200°C, a strong decrease in work function and changes in the pattern result from oxygen penetration into the bulk.     

Structural damage and its annealing response in neutron irradiated magnesium†

Abstract

Transmission electron microscopy and immersion density techniques were used to characterize the nature and extent of radiation damage in zone refined and commercial purity magnesium irradiated to 1.7 × 10²¹ neutrons/cm² (>0.1 MeV) at about 75°C. Swelling from radiation-induced voids was 1.9 and 0.7 per cent, respectively, for the high purity and commercial magnesium. This difference was caused by larger voids in the zone refined material. The voids had a non-equiaxed shape, being bounded by {0001}, {1010}, and {1011} and were flattened in ?0001?, but the larger voids were more equiaxed. There was pronounced clustering of voids on {0001} planes. The irradiation-induced dislocation structure was also clustered on the basal planes. This dislocation structure is deduced to consist of a complex tangle of 1/2 ?2023? partial dislocations and their associated stacking faults.

During postirradiation annealing, voids began to anneal out in 1 hr at 150°C and were eliminated in 1 hr at 320°C. The smaller voids as well as voids near grain boundaries disappeared first. Slow annealing of voids near some grain boundaries suggested that not all grain boundaries are equally good sinks for vacancies. Voids also became more equiaxed during annealing. Stacking faults were eliminated before the voids disappeared, and the dislocations farmed networks. Annealing treatments at 500 °C or higher caused the appearance of gas bubbles.     

Green/blue light emission and chemical feature of nanocrystalline silicon embedded in silicon-oxide thin film

2 in the range of annealing temperatures used. The PL intensity, weight of the Si⁴⁺ states, and the volume fraction of Si nanocrystals exhibit a large increase as T_a>750 °C. The PL peak position is independent of the annealing temperature (T_a). From our observations, the green/blue light emission is related to the defects. Received: 10 July 1996/Accepted: 2 April 1997     

Positron annihilation study of the vacancy clusters in ODS Fe–14Cr alloys

Abstract

Oxide dispersion strengthened Fe14Cr and Fe14CrWTi alloys produced by mechanical alloying and hot isostatic pressing were subjected to isochronal annealing up to 1400 °C, and the evolution and thermal stability of the vacancy-type defects were investigated by positron annihilation spectroscopy (PAS). The results were compared to those from a non-oxide dispersion strengthened Fe14Cr alloy produced by following the same powder metallurgy route. The long lifetime component of the PAS revealed the existence of tridimensional vacancy clusters, or nanovoids, in all these alloys. Two recovery stages are found in the oxide dispersion strengthened alloys irrespective of the starting conditions of the samples. The first one starting at T > 750 °C is attributed to thermal shrinkage of large vacancy clusters, or voids. A strong increase in the intensity of the long lifetime after annealing at temperatures in the 800–1050 °C range indicates the development of new vacancy clusters. These defects appear to be unstable above 1050 °C, but some of them remain at temperatures as high as 1400 °C, at least for 90 min.     

Structural state of III nitride layers implanted with erbium ions

The defect structure of AlGaN/GaN superlattices and GaN layers grown through vapor-phase epitaxy from organometallic compounds is investigated using x-ray diffraction analysis before and after implantation with erbium ions at an energy of 1 MeV and a dose of 3 × 10¹⁵ cm^?2, as well as after annealing. For a superlattice with a total thickness larger than the implantation depth, the satellites of the superlattice region strained under the action of ions disappear in the x-ray diffraction pattern after annealing at temperatures higher than 900°C. This suggests that the radiation-induced defects responsible for the positive deformation in the layer are annealed at these temperatures. However, annealing even at a temperature of 1050°C does not lead to complete recovery of the initial state and the positive deformation in the remaining regions is caused by residual defects. An analysis of the x-ray diffraction patterns demonstrates that, in samples with thin superlattices located at the depth corresponding to maximum radiation damage, the periodic structure that disappears after implantation at a dose of 3 × 10¹⁵ cm^?2 is not recovered even after annealing at a temperature of 1050°C. This inference is confirmed by the results of examinations with an electron microscope.     

Effects of Si and Ti impurities on electrical properties of sol–gel-derived amorphous SrTa2O6 thin films by UV/O3 treatment

Sol–gel-derived SrTa₂O₆ thin films were fabricated at a low temperature of 500 °C. To improve their leakage current properties, additional UV/O₃-assisted annealing was performed from room temperature to 290 °C. UV/O₃ treatment at 290 °C gave a very low leakage current that was six orders of magnitude lower than that of an untreated thin film. During UV/O₃-assisted annealing, Si and Ti ions diffused from the substrates into the SrTa₂O₆ thin films and occupied the Ta⁵⁺ sites, subsequently generating Si^? and Ti^?. At a heating temperature of 290 °C, large amounts of Ti ions diffused throughout the SrTa₂O₆ thin film. These Ti ions contributed to the generation of inactive combinations of $(\mathrm{Si}^{-}\mbox{--}\mathrm{V}_{\mathrm{o}}^{+})^{+}\mbox{--}\mathrm{Ti}^{-}$ and $(\mathrm{Ti}^{-}\mbox{--}\mathrm{V}_{\mathrm{o}}^{+})^{+}\mbox{--}\mathrm{Ti}^{-}$ , which greatly reduced oxygen vacancies (V_o). Thus, the leakage current was significantly reduced.     

The charge states’ conversion of the activator ions in CaF2:Eu nanophosphors

According to stationary X-ray-excited luminescence spectra and thermally stimulated luminescence spectra of CaF₂:Eu nanophosphors, it was found that Eu³⁺?→?Eu²⁺ conversion can occur during thermal annealing of fine-grained (d?=?25?nm) nanoparticles in the 200–800°C range, which is accompanied by an increase in their size within 40–189?nm. An important role of the exciton mechanism of Eu²⁺ luminescence excitation was revealed according to the temperature dependence of X-ray-excited luminescence spectra of CaF₂:Eu nanoparticles of 114?nm size. The maximum of the X-ray-excited luminescence light output of CaF₂:Eu nanophosphors in the Eu²⁺ ions’ emission band was traced out at 400–500°C annealing temperature and at the size of nanoparticles of 114–180?nm. The subsequent growth of the annealing temperatures, particularly in the 800–1000°C range, causes the reduction of X-ray-excited luminescence light output because of the increment of lattice defects’ concentration due to a sharp increase in the size of nanoparticles and their agglomeration.     

Effect of annealing temperature on the structure of pyrolysates of diphthalocyanines of rare-earth elements: Neutron research

Small-angle neutron scattering is used to study the structure of carbon matrices—the pyrolysis products of diphthalocyanines with embedded metal atoms (Y, La, and Ce), synthesized at annealing temperatures of 800–1700°C. It is shown that the structure of the porous matrix on the scale of ～10⁰–10² nm is characterized by a level of small pores (3–10 nm in radius) and the next level of the structure is associated with the formation of their aggregates (above 100 nm in size). The quantity and size of the scattering objects increases sharply at annealing temperatures above 1000°C. The results are consistent with X-ray diffraction data.     

Effects of annealing on the luminescent properties from defects formed in electron-irradiated GaN

The effects of annealing on the luminescence properties of electron-irradiated GaN were investigated by photoluminescence (PL), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Our results indicate that the yellow luminescence (YL) remains disappear after all annealing treatments and shows a non-linear dependence on the annealing temperature up to 800 °C. The annealing process can be divided into two main stages associated with irradiation defects. At annealing temperatures up to 600 °C, the behavior of YL can be attributed to the net effects of V_GaO_N complex formation caused by the migration of gallium vacancies (V_Ga) and V_GaO_N complex dissociation due to the disappearance of gallium vacancies. At annealing temperatures approaching 800 °C, the incorporation of carbon into the group-V sublattice becomes the dominant factor in the appearance of YL. In addition, experimental results of PL and SEM show that a small proportion of irradiation damage still exists in GaN after annealing at 800 °C.     

Nitrogen centers in GaP produced by hot implantation

Backscattering yields of 1.5 MeV?He⁺ ions and low temperature photoluminescence (PL) spectra were measured in GaP crystals implanted with 200 keV?N⁺ ions as functions of ion-dose, temperature during implantation and annealing temperature after implantation. Backscattering results indicate that hot implantation at 500°C greatly reduces radiation damage. The PL intensities of NN lines become maximum in the sample implanted with N⁺ ions of 3 × 10¹⁴cm^?2 at 500°C, and annealed at 1000°C for 1 hr with aluminum glass. The PL intensity is comparable to that of the nitrogen-doped sample during liquid phase epitaxy which is widely accepted as the best method of introducing nitrogen into GaP crystals. In the case of 500°C—hot implantation, the radiation damage produced during implantation is annealed out at 700 ~ 800°C and the implanted nitrogen substitutes for the phosphorous sites after annealing at 900 ~ 1000°C. Some kinds of defects or strains remain around the NN centers even in implanted samples with a maximum PL efficiency. These defects or strains don't seem to reduce the PL efficiency. In the case of room temperature implantation, PL efficiency decreases to one-hundredth or one-thousandth due to the formation of the non-crystalline state compared with hot implantation.     

Development of conductive transparent indium tin oxide (ITO) thin films deposited by direct current (DC) magnetron sputtering for photon-STM applications

Highly conductive and transparent indium tin oxide (ITO) thin films, each with a thickness of 100 nm, were deposited on glass and Si(100) by direct current (DC) magnetron sputtering under an argon (Ar) atmosphere using an ITO target composed of 95% indium oxide and 5% tin oxide for photon-STM use. X-ray diffraction, STM observations, resistivity and transmission measurements were carried out to study the formation of the films at substrate temperatures between 40 and 400 °C and the effects of thermal annealing in air between 200 and 400 °C for between1 and 5 h. The film properties were highly dependent on deposition conditions and on post-deposition film treatment. The films deposited under an Ar atmosphere pressure of ∼1.7×10^-3 Torr by DC power sputtering (100 W) at substrate temperatures between 40 and 400 °C exhibited resistivities in the range 3.0–5.7×10^-5 Ω m and transmissions in the range 71–79%. After deposition and annealing in air at 300 °C for 1 h, the films showed resistivities in the range 2.9–4.0×10^-5 Ω m and transmissions in the range 78–81%. Resistivity and transmission measurements showed that in order to improve conductive and transparent properties, 2 h annealing in air at 300 °C was necessary. X-ray diffraction data supported the experimental measurements of resistivity and transmission on the studies of annealing time. The surface roughness and film uniformity improve with increasing substrate temperature. STM observations found the ITO films deposited at a substrate temperature of 325 °C, and up to 400 °C, had domains with crystalline structures. After deposition and annealing in air at 300 °C for 1 h the films still exhibited similar domains. However, after deposition at substrate temperatures from 40 °C to 300 °C, and annealing in air at 300 °C for 1 h, the films were shown to be amorphous. More importantly, the STM studies found that the ITO film surfaces were most likely to break after deposition at a substrate temperature of 325 °C and annealing in air at 300 °C for 2 or 3 h. Such findings give some inspiration to us in interpreting the effects of annealing on the improvement of conductive and transparent properties and on the transition of phases. In addition, correlations between the conductive/transparent properties and the phase transition, the annealing time and the phase transition, and the conductive/transparent properties and the annealing time have been investigated. Received: 10 July 2000 / Accepted: 27 October 2000 / Published online: 9 February 2001     

Self-diffusion in α-Fe2O3 natural single crystals

Measurements of¹⁸O self-diffusion in hematite (Fe₂O₃) natural single crystals have been carried out as a function of temperature at constant partial pressure a_{O 2}=6.5·10^?2 in the temperature range 890 to 1227 °C. The a_{O 2} dependence of the oxygen self-diffusion coefficient at fixed temperature T=1150 °C has also been deduced in the a_{O 2} range 4.5·10^?4 - 6.5·10^?1. The concentration profiles were established by secondary-ion mass spectrometry; several profiles exhibit curvatures or long tails; volume diffusion coefficients were computed from the first part of the profiles using a solution taking into account the evaporation and the exchange at the surface. The results are well described by $$D_O \left( {{{cm^2 } \mathord{\left/ {\vphantom {{cm^2 } s}} \right. \kern-\nulldelimiterspace} s}} \right) = 2.7 \cdot 10^8 a_{O_2 }^{ - 0.26} \exp \left( { - \frac{{542\left( {{{kJ} \mathord{\left/ {\vphantom {{kJ} {mol}}} \right. \kern-\nulldelimiterspace} {mol}}} \right)}}{{RT}}} \right)$$ From fitting a grain boundary diffusion solution to the profile tails, the oxygen self-diffusion coefficient in sub-boundaries has been deduced. They are well described by $$D''_O \left( {{{cm^2 } \mathord{\left/ {\vphantom {{cm^2 } s}} \right. \kern-\nulldelimiterspace} s}} \right) = 3.2 \cdot 10^{25} a_{O_2 }^{ - 0.4} \exp \left( { - \frac{{911\left( {{{kJ} \mathord{\left/ {\vphantom {{kJ} {mol}}} \right. \kern-\nulldelimiterspace} {mol}}} \right)}}{{RT}}} \right)$$ Experiments performed introducing simultaneously¹⁸O and⁵⁷Fe provided comparative values of the self-diffusion coefficients in volume: iron is slower than oxygen in this system showing that the concentrations of atomic point defects in the iron sublattice are lower than the concentrations of atomic point defects in the oxygen sublattice. The iron self-diffusion values obtained at T>940 °C can be described by $$D_{Fe} \left( {{{cm^2 } \mathord{\left/ {\vphantom {{cm^2 } s}} \right. \kern-\nulldelimiterspace} s}} \right) = 9.2 \cdot 10^{10} a_{O_2 }^{ - 0.56} \exp \left( { - \frac{{578\left( {{{kJ} \mathord{\left/ {\vphantom {{kJ} {mol}}} \right. \kern-\nulldelimiterspace} {mol}}} \right)}}{{RT}}} \right)$$ The exponent - 1/4 observed for the oxygen activity dependence of the oxygen self-diffusion in the bulk has been interpreted considering that singly charged oxygen vacancies V _O ^? are involved in the oxygen diffusion mechanism. Oxygen activity dependence of iron self-diffusion is not known accurately but the best agreement with the point defect population model is obtained considering that iron self-diffusion occurs both via neutral interstitals Fe _x ⁱ and charged ones.     

Thermally activated crystallization of Nb2O5 grown on Pt electrode

The influence of the local crystallographic orientation of the polycrystalline bottom platinum electrode on the crystallization of niobium pentoxide thin films during their rapid thermal annealing was investigated by X-ray diffraction, X-ray reflectivity and transmission electron microscopy. The Nb₂O₅ thin films under study were reactively sputtered in a mixed O₂/Ar atmosphere and subsequently subjected to the annealing in argon atmosphere at temperatures ranging from 500 ^°C to 700 ^°C. The X-ray diffraction confirmed a transition from the amorphous niobium oxide to the crystalline orthorhombic Nb₂O₅ for temperatures between 500 ^°C and 600 ^°C. The X-ray reflectivity measurements showed that the crystallization process was accompanied by a continuous increase of the electron density in Nb₂O₅ and by a rapid increase of the surface roughness at 700 ^°C. It was further observed by transmission electron microscopy that Nb₂O₅ crystallizes selectively and that the crystalline domains of Nb₂O₅ possess a strong orientation relationship to the platinum from the bottom electrode. The orientation relationship $(\bar{1} 1 1)_{\mathrm{Pt}}\,{\parallel}\, (\bar{1} \bar{6}0)_{\mathrm{Nb}_{2}\mathrm{O}_{5}}$ was identified as the most beneficial one for crystallization of Nb₂O₅.     

Investigation of silicon doped by zinc ions with a large dose

The formation of nanoparticles in СZn-Si(100) implanted with ⁶⁴Zn⁺ ions using a dose of 5 × 10¹⁶ cm^–2 and an energy of 50 keV at room temperature with subsequent thermal processing in oxygen at temperatures ranging from 400 to 900°C is studied. The surface topology is investigated with scanning electron (in the secondary emission mode) and atomic force microscopes. The structure and composition of the near-surface silicon layer are examined using a high-resolution transmission electronic microscope fitted with a device for energy dispersive microanalysis. An amorphized near-surface Si layer up to 130 nm thick forms when zinc is implanted. Amorphous zinc nanoparticles with an average size of 4 nm are observed in this layer. A damaged silicon layer 50 nm thick also forms due to radiation defects. The metallic zinc phase is found in the sample after low-temperature annealing in the range of 400–600°C. When the annealing temperature is raised to 700°C, zinc oxide ZnO phase can form in the near-surface layer. The complex ZnO · Zn₂SiO₄ phase presumably emerges at temperatures of 800°C or higher, and zinc-containing nanoparticles with lateral sizes of 20–50 nm form on the sample’s surface.     

Annealing embrittlement of Fe78Si9B13 (METGLAS-2605S2)

The ductile to brittle transition that occurs in amorphous Fe₇₈Si₉B₁₃ (METGLAS-2605S2) has been investigated using mechanical measurements over the temperature range 250–370 °C. The fracture toughness values, K _Ic , have been determined for a range of annealing times (5–30 min) and cooling rates of 15–45 °C/min. A pronounced ductile to brittle transition is observed around 310(10) °C although no obvious structural changes are evident as indicated by x-ray diffraction. Comparison of transmission and back-scattered conversion electron ⁵⁷Fe Mössbauer spectra for the bulk as-received ribbon in the ductile state ( $K_{Ic}=52~{\rm MPa} \cdot \sqrt{m}$ ) and the ribbon annealed to the brittle state ( $K_{Ic}\sim10~{\rm MPa} \cdot \sqrt{m}$ ) indicates magnetic texture effects in both the bulk and on the surface of these amorphous ribbons, related to the magnetostriction resulting from the quenched-in stress during the ribbon production process, and the ensuing stress-relief upon annealing.     

Investigation of structural transformations in nanophase titanium dioxide by Raman spectroscopy

2 ) prepared by a colloidal chemistry method. The evolution of the anatase phase upon annealing was characterized by frequency downshift, intensity increase, and linewidth sharpening of the lowest-frequency E_g mode. The rutile phase was shown to be stabilized at temperatures below 350 °C and was postulated to reside in the surface region of the nanophase. The beginning and ending temperatures for the anatase–rutile transformation in the nanophase were found to be lower than those in single crystals or polycrystalline powders. The microscopic mechanism of the phase transformation was analyzed and the surface effect was suggested. An anomalous phenomenon of amorphization was also detected at the end of the anatase–rutile transformation in the nanophase TiO₂. Received: 5 November 1997/Accepted: 6 November 1997     

Characterization of silicon doped with sodium upon high-voltage implantation

The depth distribution profiles of sodium atoms in silicon upon high-voltage implantation (ion energy, 300 keV; implantation dose, 5 × 10¹⁴ and 3 × 10¹⁵ cm ^?2) are investigated before and after annealing at temperatures in the range T _ann = 300–900°C (t _ann = 30 min). Ion implantation is performed with the use of a high-resistivity p-Si (ρ= 3–5 kΩ cm) grown by floating-zone melting. After implantation, the depth distribution profiles are characterized by an intense tail attributed to the incorporation of sodium atoms into channels upon their scattering from displaced silicon atoms. At an implantation dose of 3 × 10¹⁵ ions/cm², which is higher than the amorphization threshold of silicon, a segregation peak is observed on the left slope of the diffusion profile in the vicinity of the maximum after annealing at a temperature T _ann = 600°C. At an implantation dose of 5 × 10¹⁴ ions/cm², which is insufficient for silicon amorphization, no similar peak is observed. Annealing at a temperature T _ann = 700°C leads to a shift of the profile toward the surface of the sample. Annealing performed at temperatures T _ann ≥ 800°C results in a considerable loss of sodium atoms due to their diffusion toward the surface of the sample and subsequent evaporation. After annealing, only a small number of implanted atoms that are located far from the region of the most severe damages remain electrically active. It is demonstrated that, owing to the larger distance between the diffusion source and the surface of the sample, the superficial density of electrically active atoms in the diffusion layer upon high-voltage implantation of sodium ions is almost one order of magnitude higher than the corresponding density observed upon low-voltage implantation (50–70 keV). In this case, the volume concentration of donors near the surface of the sample increases by a factor of 5–10. The measured values of the effective diffusion parameters of sodium at annealing temperatures in the range T _ann = 525–900°C are as follows: D ₀ = 0.018 cm²/s and E _a = 1.29 eV/kT. These parameters are almost identical to those previously obtained in the case of low-voltage implantation.     

Effects of annealing temperature on the structure, photoluminescence and ferromagnetism properties of Cr-implanted ZnO nanowires

Room temperature ferromagnetism was observed in Cr-implanted ZnO nanowires annealed at 500, 600, and 700 °C. The implantation dose for Cr ions was 1×10¹⁶ cm^?2, while the implantation energies were 100 keV. Except for ZnO (100), (002), and (200) orientations, no extra diffraction peaks from Cr-related secondary phase or impurities were observed. With the increasing of annealing temperatures, the intensity of the peaks increased while the FWHM values decreased. The Cr 2p_1/2 and 2p_3/2 peaks, with a binding energy difference of 10.6 eV, appear at 586.3 and 575.7 eV, can be attributed to Cr³⁺ in ZnO nanowires. For the Cr-implanted ZnO nanowires without annealing, the band energy emission disappears and the defect related emission with wavelength of 500–700 nm dominates, which can be attributed to defects introduced by implantation. Cr-implanted ZnO nanowires annealed at 500 °C show a saturation magnetization value of over 11.4×10^?5 emu and a positive coercive field of 67 Oe. The origin of ferromagnetism behavior can be explained on the basis of electrons and defects that form bound magnetic polarons, which overlap to create a spin-split impurity band.     

A novel intrinsically proton conducting star-shaped imidazole terminated oligomers

In this paper, intrinsically proton conducting imidazole-terminated oligomers were synthesized by tethering imidazole units via flexible ethylene oxides (EO) chain onto 1,3,5-benzenetricarbonyl chloride (TMA). The structure of the resulting material was confirmed by FT-IR; ¹H-NMR spectrometer and compositions were obtained by elemental analysis. Thermogravimetry results showed that the materials are thermally stable up to approximately 160 °C. Differential scanning calorimeter studies were performed to study the influence of the length of EO units on the glass transition temperatures of the materials. The conductivity isotherms exhibit Vogel–Tamman–Fulcher behavior with a maximum proton conductivity of at 110 °C for TMA-(Peg₆₀₀-Imi)₃.