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.     

Structural relaxation in the CoP-CoNiP system upon low-temperature annealing

The atomic structure of alloys in the CoP-CoNiP system in the initial state and its behavior upon low-temperature annealing is investigated. It is shown that structural relaxation starts at temperatures of 150–200°C and results in local atomic ordering at the network boundaries. Crystals 2–5 nm in size start to undergo nucleation at the boundaries of structural heterogeneities when heated further to 250–300°C. The nanocrystal structure corresponds to the metastable phase delta-Co (ICSD 42684) and the unknown phase Co_{1 ? x} P _x . The estimated diffusion coefficient for CoP alloy is 10^?14 m² s^?1, according to the experimental data.     

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.     

Electron microscopy studies of void swelling and annealing of voids in aluminium irradiated with aluminium ions

Abstract

MgO single crystals implanted with Au⁺ ions (180 keV, 6 10¹⁶-10¹⁷ ions cm^?2) and annealed at temperatures between 25°C and 1100°C, have been analysed—by optical spectrophotometry—by Rutherford back-scattering (to confirm the effective presence and to study the distribution profile of Au atoms), and by TEM and X-ray diffraction (to identify the phases precipitated by thermal treatment).

Thermal annealing between 550°C and 1100°C produced an optical absorption band located between 565 nm and 600 nm. This band can be attributed to a fee Au precipitate with diameter varying from 50 to 200 Å. Larger metallic colloids 1000 Å are in simple orientation with the matrix.

Annealing at temperatures higher than 500°C produces a supplementary optical absorption located at 425 nm. This band can be attributed to Au plasma resonance.

After annealing for 15 min at 1100°C, a new phase is detected by X-ray diffraction and TEM and identified as Au₃Mg alloy with hexagonal structure.     

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     

Radiation hardening in Zircaloy-2

Annealed Zircaloy-2 was exposed to fast neutron fluences in the range 0.46 to 6.71 × 10¹⁹ nvt, E > 1 MeV, at temperatures of up to 450°C. The level of radiation hardening, as measured by the change in yield stress after irradiation, increased with irradiation temperature at least up to 380°C.

Post-irradiation annealing treatments showed that radiation anneal hardening occurred after irradiation at temperatures up to 325°C. After irradiation at 375°C, annealing treatments did not produce a further increase in the yield stress above that produced by the irradiation, however the radiation hardening persisted to 450°C. The uniform strain tended to decrease as the amount of radiation anneal hardening increased and as the fast neutron fluence increased above ～5 × 10¹⁸ nvt, E > 1 MeV.

The effects of irradiation temperature and post-irradiation annealing on the yield stress and on uniform strain are explained in terms of the strengthening of radiation damage defect clusters and their increased effectiveness to impede dislocation movement.     

Growth and magnetic behavior of bismuth substituted yttrium iron garnet nanoparticles

Crystal growth and the magnetic properties of bismuth substituted yttrium iron garnet (Bi-YIG) nanoparticles were studied with particular focus on the bismuth composition dependence of the magnetic properties of the particles and the effects of annealing on the garnet phase formation. The Bi-YIG nanoparticles of 47–67 nm in size can be chemically synthesized when they are annealed at 650–850 °C. Both the lattice constant and the magnetization of the garnet nanoparticles linearly increase when the bismuth composition in the Bi-YIG particles increases. We have found that chemically synthesized nanoparticles transform from the amorphous to the garnet phase when annealed at temperatures below 650 °C, while the onset of magnetic moment of iron in the garnet nanoparticles is observed slightly above 650 °C. According to Mössbauer effect measurements, the hyperfine fields of ⁵⁷Fe at the tetrahedral and octahedral sites in the garnet are 39 and 48 T, respectively.     

Lattice site location and electronic structure of Te in GaAs

High purity <100> wafers of GaAs were implanted with radioactive^129mTe and stable¹²⁸Te at 110 keV to total doses of 2×10¹⁴ and 2×10¹⁵ Te/cm² respectively and studied with RBS/ channeling and Mössbauer spectroscopy on the 27.8 keV level of¹²⁹I. After implantation and/or annealing at temperatures between 200–300°C the Mössbauer spectra are dominated by a single line. Channeling reveals an appreciable residual damage in the host lattice, but also points to a substitutional position of the Te atoms. After annealing above ≌500°C, where nearly complete lattice damage recovery is obtained, the Te atoms become defect-associated. The results clearly point to the formation of Te_As?V_Ga complexes.     

Effect of annealing on the electronic parameters of Au/poly(ethylmethacrylate)/n-InP Schottky diode with organic interlayer

A thin poly(ethylmethacrylate) (PEMA) layer is deposited on n-InP as an interlayer for electronic modification of Au/n-InP Schottky structure. The electrical properties of Au/PEMA/n-InP Schottky diode have been investigated by current–voltage (I–V) and capacitance–voltage (C–V) measurements at different annealing temperatures. Experimental results show that Au/PEMA/n-InP structure exhibit a good rectifying behavior. An effective barrier height as high as 0.83 eV (I–V) and 1.09 eV (C–V) is achieved for the Au/PEMA/n-InP Schottky structure after annealing at 150 °C compared to the as-deposited and annealed at 100 and 200 °C. Modified Norde's functions and Cheung method are also employed to calculate the barrier height, series resistance and ideality factors. Results show that the barrier height increases upon annealing at 150 °C and then slightly decreases after annealing at 200 °C. The PEMA layer increases the effective barrier height of the structure as this layer creates a physical barrier between the Au metal and the n-InP. Terman's method is used to determine the interface state density and it is found to be 5.141 × 10¹² and 4.660 × 10¹² cm^?2 eV^?1 for the as-deposited and 200 °C annealed Au/PEMA/n-InP Schottky diodes. Finally, it is observed that the Schottky diode parameters change with increasing annealing temperature.     

Synthesis of nano-polycrystalline diamond from glassy carbon at pressures up to 25 GPa

ABSTRACT

Nano-polycrystalline diamond (NPD) with various grain sizes has been synthesized from glassy carbon at pressures 15–25?GPa and temperatures 1700–2300°C using multianvil apparatus. The minimum temperature for the synthesis of pure NPD, below which a small amount of compressed graphite was formed, significantly increased with pressure from ～1700°C at 15?GPa to ～1900°C at 25?GPa. The NPD having grain sizes less than ～50?nm was synthesized at temperatures below ～2000°C at 15?GPa and ～2300°C at 25?GPa, above which significant grain growth was observed. The grain size of NPD decreases with increasing pressure and decreasing temperature, and the pure NPD with grain sizes less than 10?nm is obtained in a limited temperature range around 1800–2000°C, depending on pressure. The pure NPD from glassy carbon is highly transparent and exhibits a granular nano-texture, whose grain size is tunable by selecting adequate pressure and temperature conditions.     

Evolution of the spectral characteristics upon annealing of lithium borate glasses containing europium and aluminum

The spectral and structural characteristics of lithium borate glasses containing europium and aluminum have been investigated upon annealing at different temperatures. It has been found that the spectral characteristics of the studied system change nonmonotonically with an increase in the annealing temperature. After annealing at a temperature of 600°C, the luminescence spectra of the glasses exhibit broad structureless bands that are specific for the amorphous phase containing Eu³⁺ ions. Then, after annealing at T = 700°C, narrow lines appear in the wavelength ranges 585–595 and 610–620 nm, which correspond to the luminescence of the Eu(BO₂)₃ and EuAl₃(BO₃)₄ borates. A further increase in the annealing temperature (T = 800–900°C) leads to the disappearance of europium aluminum borate. In the luminescence spectra of these samples, there are narrow bands in the wavelength range λ = 585–595 nm, which are typical of europium metaborate. Finally, at a temperature of 1050°C, these bands disappear and narrow lines appear again in the wavelength range 610–620 nm, which are characteristic of the EuAl₃(BO₃)₄ borate. Thus, the temperature annealing makes it possible to purposely change the spectral characteristics of the studied system in the wavelength range 590–615 nm.     

Charge states of the activator and size effects in BaF2: Eu nanophosphors

ABSTRACT

According to the spectra of stationary X-ray excited luminescence (XEL) of BaF₂: Eu nanophosphors at 80 and 294 K, it was revealed that the thermal annealing of fine-grained nanoparticles (d?=?35?nm) in the range of 400–1000°C, which is accompanied by an increase of their sizes in the range of 58–120?nm, does not result in effective changes of the charge state of Eu^{3 +} → Eu^{2 +} activator, in contrast to CaF₂: Eu nanoparticles. The maximum light output of X-ray excited luminescence of BaF₂: Eu nanophosphors in the 590?nm emission band of Eu³⁺ ion was observed at an annealing temperature of 600°C with the average size of nanoparticles 67?nm. The subsequent growth of annealing temperatures, especially in the range of 800–1000°C, causes decrease in the light output of X-ray excited luminescence due to the increase of defect concentration in the lattice as a result of sharp increase of nanoparticle sizes and their agglomeration. In BaF₂: Eu nanoparticles of 58?nm size, according to the thermostimulated luminescence (TSL) spectrum, transformation of Eu³⁺ → Eu²⁺ under the influence of long-time X-ray irradiation was revealed for the peak of 151?K. Thus, X-ray excited luminescence spectra of BaF₂: Eu nanophosphors are formed predominantly due to the emission of Eu³⁺ ions, while emission of Eu²⁺ ions is observed in the TSL spectra.     

Recrystallization of hexagonal silicon carbide after gold ion irradiation and thermal annealing

Silicon carbide (SiC) single crystals with the 6H polytype structure were irradiated with 4.0-MeV Au ions at room temperature (RT) for increasing fluences ranging from 1?×?10¹² to 2?×?10¹⁵ cm^?2, corresponding to irradiation doses from ~0.03 to 5.3 displacements per atom (dpa). The damage build-up was studied by micro-Raman spectroscopy that shows a progressive amorphization by the decrease and broadening of 6H-SiC lattice phonon peaks and the related growth of bands assigned to Si–Si and C–C homonuclear bonds. A saturation of the lattice damage fraction deduced from Raman spectra is found for ~0.8?dpa (i.e. ion fluence of 3?×?10¹⁴ cm^?2). This process is accompanied by an increase and saturation of the out-of-plane expansion (also for ~0.8?dpa), deduced from the step height at the sample surface, as measured by phase-shift interferometry. Isochronal thermal annealing experiments were then performed on partially amorphous (from 30 to 90%) and fully amorphous samples for temperatures from 200 °C up to 1500 °C under vacuum. Damage recovery and densification take place at the same annealing stage with an onset temperature of ~200 °C. Almost complete 6H polytype regrowth is found for partially amorphous samples (for doses lower than 0.8 dpa) at 1000 °C, whereas a residual damage and swelling remain for larger doses. In the latter case, these unrelaxed internal stresses give rise to an exfoliation process for higher annealing temperatures.     

Secondary defects in low-energy As-implanted Si

14 /cm² dose of As ions followed by both isochronal and isothermal annealing. The elementary defects generated first during solid-phase epitaxial recovery of implantation-induced amorphous layers at temperatures of 550 °C and/or 600 °C are {311} defects 2–3 nm long. They are considered to be transformed into {111} and {100} defects after annealing at temperatures higher than 750 °C. These secondary defects show the opposite annealing behavior to the dissolution and growth by the difference of their depth positions at 800 °C. This phenomenon is explained by the diffusion of self-interstitials contained in defects. With regard to the formation and dissolution of defects, there is no significant difference between the effects of rapid thermal annealing (950 °C for 10 s) and furnace annealing (800 °C for 10 min). Received: 14 November 1997/Accepted: 16 November 1997     

Structural characterisation of the silica and alumina Zener pinning phases in nanocrystalline CeO2 by 29Si and 27Al nuclear magnetic resonance

Nanocrystalline CeO₂ samples have been manufactured using sol-gel techniques, containing either 15 % silica or 10 % alumina by weight to restrict growth of the ceria nanocrystals during annealing by Zener pinning. ²⁹Si and ²⁷Al MAS NMR have been used to investigate the structure of these pinning phases over a range of annealing temperatures up to 1000 °C, and their effect on the CeO₂ morphology has been studied using electron microscopy. The silica pinning phase resulted in CeO₂ nanocrystals of average diameter 19 nm after annealing at 1000 °C, whereas the alumina pinned nanocrystals grew to 88 nm at the same temperature. The silica pinning phase was found to contain a significant amount of inherent disorder indicated by the presence of lower n Qⁿ species even after annealing at 1000 °C. The alumina phase was less successful at restricting the growth of the ceria nanocrystals, and tended to separate into larger agglomerations of amorphous alumina, which crystallised to a transition alumina phase at higher temperatures.     

Peculiarities of structural phase and elastic stress states of superhard TiN-based nanocomposite coatings

A new concept of designing nanocomposite coatings is proposed. The concept consists in microstructural self-organization through simultaneous nucleation of islands of different mutually insoluble or slightly soluble phases at the stage of coating formation. Physical principles on which to select compositions of the coatings were developed and were experimentally verified on multicomponent nanocomposite coatings. With a Sprut magnetron arc plasma complex, superhard (H _μ > 40 GPa) multicomponent nanocomposite coatings of the system Ti-Al-Si-Cr-Ni-Cu-O-C-N were obtained. The peculiarities of structural phase and elastic stress states of the multicomponent coatings before and after annealing at a temperature of up to 1000 °C were studied by transmission electron microscopy, X-ray diffraction analysis, microhardness measurements and scratch tests. The study reveals a wide range of lattice bending-torsion (up to 200° μm^?1) of nanosized (less than 30 nm) coherent scattering regions in the two-level coating structure and of individual (up to 15 nm) TiN nanocrystals. Annealing of the coatings causes the two-level grain structure to relax with the formation of TiN-based nanocrystals of size less than 30–40 nm and with a decrease in lattice bending-torsion down to 40°–50° μm^?1. Comparative analysis of acoustic emission signals and tracks of the multicomponent and TiN coatings in scratch tests points to an increase in fracture ductility in the multicomponent coatings.     

Correlation between luminescent properties and structure organization in AlGaN/GaN superlattices annealed after erbium ion implantation

The evolution of the structure organization of MOCVD-grown AlGaN/GaN superlattices subjected to erbium ion implantation with an energy of 1 MeV and dose of 3 × 10¹⁵ cm^?2 and subsequent annealing is correlated with their photoluminescent properties. The structure organization is quantitatively estimated using parameter Δ (degree of violation of local symmetry), which is found via multifractal analysis of surface morphology patterns obtained with atomic force microscopy. It is shown that the implantation not only causes Ga segregation on the surface, but also changes the structure organization, which shows up in the finer grain structure compared with the starting one and disordering, as well as in an increase in Δ. As the annealing temperature rises from 700 to 800°C, Δ declines, indicating that the structure organization is improved, and the intensity of the dominating photoluminescence peak due to Er³⁺ ions (1.542 μm) grows. With a further increase in the annealing temperature to 1050°C, the structure organization degrades, domains get larger, voids 100–200 nm deep form, and the photoluminescence intensity drops. The formation of voids during high-temperature annealing is also substantiated by data for 230-keV proton scattering. It is thus established that the improvement of the superlattice structure organization activates erbium and causes the erbium-ion-related luminescence intensity to grow.     

Ion beam shaping of embedded metal nanoparticles by Si+ ion irradiation

Fine Co and Pt nanoparticles are nucleated when a silica sample is implanted with 400 keV Co⁺ and 1370 keV Pt⁺ ions. At the implanted range, Co and Pt react to form small Co _x Pt_(1?x) nanoparticles during Si⁺ ion irradiation at 300 °C. Thermal annealing of the pre-implanted silica substrate at 1000 °C results in the formation of spherical nanoparticles of various sizes. When irradiated with Si⁺ ions at 300 °C, particles in the size range of 5–17 nm undergo rod-like shape transformation with an elongation in the direction of the incident ion beam, while those particles in the size range of 17–26 nm turn into elliptical shape. Moreover, it is suspected that very big nanoparticles (size >26 nm) decrease in size, while small nanoparticles (size <5 nm) do not undergo any transformation. During Si⁺ ion irradiation, the crystalline nature of the nanoparticles is preserved. The results are discussed in the light of the thermal spike model.     

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.     

Phase transformation of Ni/Si thin films induced by nanoindentation and annealing

Thin Ni/Si films are prepared by depositing a Ni layer with a thickness of 100 nm on a Si (100) substrate. The as-deposited thin-film specimens are indented to a maximum depth of 500 nm using a nanoindentation technique and are then annealed at temperatures of 200°C, 300°C, 500°C and 800°C for 2 min. The microstructural changes and phases induced in the various specimens are observed using transmission electron microscopy (TEM) and micro-Raman scattering spectroscopy (RSS). Based on the load-displacement data obtained in the nanoindentation tests, the hardness and Young’s modulus of the as-deposited specimens are found to be 13 GPa and 177 GPa, respectively. The microstructural observations reveal that the nanoindentation process prompts the transformation of the indentation-affected zone of the silicon substrate from a diamond cubic structure to a mixed structure comprising amorphous phase and metastable Si III and Si XII phases. Following annealing at temperatures of 200∼500°C, the indented zone contains either a mixture of amorphous phase and Si III and Si XII phases, or Si III and Si XII phases only, depending on the annealing temperature. In addition, the annealing process prompts the formation of nickel silicide phases at the Ni/Si interface or within the indentation zone. The composition of these phases depends on the annealing temperature. Specifically, Ni₂Si is formed at a temperature of 200°C, NiSi is formed at a temperature of 300°C and 500°C, and NiSi₂ is formed at 800°C.