Dimpling—A new manifestation of ion-produced lattice damage

Abstract

Bombardment of thin (1–10 μ) single crystal targets with energetic ion beams has been found to result in macroscopic distortion of the thin film in the bombarded region. This effect, which has been euphemistically termed a ‘dimple’, is readily observed with the naked eye even at relatively low particle fluence. A useful first-order model has been developed which interprets the dimpling as an expansion of the bombarded region. For very thin samples, this expansion can be accommodated by bowing of the crystal out of the original crystal plane. For this simple model, the fractional expansion is proportional to (δ/d)² where δ is the maximum displacement from the original crystal plane and d is the diameter of the bombarded area. This measurement allows expansioh to be determined with a sensitivity comparable to or better than the most sensitive existing methods.

For silicon about 3 μ thick bombarded by 1.8 MeV He ions, the expansion increases essentially linearly with fluence at the lowest fluence (below about 10¹⁵ to 10¹⁴ cm^?2). In this region about 0.001 atomic volumes are added per incident ion. As the fluence is increased, the apparent expansion begins to increase more rapidly than linearly but approaches a saturation value at the highest fluence (about 10¹⁸ cm^?2). The effect of particle flux, incident energy, and bombardment temperature is discussed as well as some preliminary results on C ion produced dimples in Si and the behavior of Ge samples.

Thirty-minute isochronal annealing of silicon samples irradiated with He ions at room temperature shows reverse annealing for temperatures up to about 200–300°C. The dimple begins to anneal at 300°C and disappears after annealing to 600–700°C.

After irradiation, the dimpled region absorbs light more strongly in the visible and near IR region. This disappears with annealing before the dimple itself completely disappears and is felt to be largely due to scattering from defect clusters.     

Effect of 30 Mev Li 3+ ion and 8 MeV electron irradiation on n-channel MOSFETs

The effect of 30 v MeV Li 3+ ion and 8 v MeV electron irradiation on the threshold voltage ( V TH ), the voltage shift due to interface trapped charge ( j V Nit ), the voltage shift due to oxide trapped charge ( j V Not ), the density of interface trapped charge ( j N it ), the density of oxide trapped charge ( j N ot ) and the drain saturation current ( I D v Sat ) were studied as a function of fluence. Considerable increase in j N it and j N ot , and decrease in V TH and I D v Sat were observed in both types of irradiation. The observed difference in the properties of Li 3+ ion and electron irradiated MOSFETs are interpreted on the basis of energy loss process associated with the type of radiation. The study showed that the 30 v MeV Li 3+ ion irradiation produce more damage when compared to the 8 v MeV electron irradiation because of the higher electronic energy loss value. High temperature annealing studies showed that trapped charge generated during ion and electron irradiation was annealed out at 500 v °C.     

Luminescence studies of Co implanted sapphires

Sapphire single crystals implanted with different fluences of cobalt and subjected to annealing treatments in vacuum and in air during 1 v h at 1000 v C were studied by optical and structural techniques. At room temperature the absorption mainly occurs in the ultraviolet (UV) being the luminescence dominated by a UV/blue broad emission band and a highly structured red emission. Structural analysis indicates that metallic precipitates, CoAl 2 O 4 and CoO phases are present in the implanted and annealed samples depending either on the fluence and on the annealing atmosphere. The observed luminescence cannot be correlated with intra-ionic Co 2+ and Co 3+ in an Al 3+ site in the sapphire lattice and a tentative assignment of the observed emission lines to the presence of aggregates is made.     

Luminescence sensitivity changes of quartz by bleaching,annealing and UV exposure

The sensitivities of quartz luminescence signals to dose were studied after ionizing irradiation, ultraviolet (UV) exposure and different annealing conditions. The relationship between the 110 v °C thermoluminescence (TL) and optically stimulated luminescence (OSL) were studied on the same aliquot by looking at the ratio of both signals created by a test dose. It is suggested that the sensitivity changes of both signals are closely related, but not identical. Significant differences are observed when annealing to temperatures higher than 500 v °C. A modified model was proposed to interpret the observations. The similarity is interpreted as the same R hole centers are shared by both signals, whereas 110 v °C TL only uses additional R hole centers. Dramatic changes in luminescence sensitivity for quartz relate to the phase changes.     

Mechanism of long-lasting phosphorescence of Eu 2+ in melilite

UV excitation for several Eu 2+ -doped melilite crystals, Eu 2+ :Ca 2 Al 2 SiO 7 (CASM), Eu 2+ :CaSrAl 2 SiO 7 (CSASM), and Eu 2+ :Sr 2 Al 2 SiO 7 (SASM) produces long-lasting phosphorescence (1-10 2 v s) from Eu 2+ ions besides the intrinsic Eu 2+ luminescence. The distribution of the radiative decay rates is due to the recombination of distant pairs of trapped electrons and holes in the crystals. The intensities of the phosphorescence for these crystals were measured as functions of temperature and time. The most intense phosphorescence was obtained from the Eu 2+ : SASM crystal. The decay curves measured for Eu 2+ :SASM below 400 v K fit t m n ( n h 1). This fact shows that the recombination of the distant pairs occurs through tunneling below 400 v K. The temperature dependence of the intensities integrated in a time domain obeys the Arrhenius's equation with two thermal activation energies including radiative and non-radiative processes. These results suggest that holes and electrons recombine radiatively at Eu 2+ sites in the SASM crystal through thermal hopping and tunneling. On the other hand, Eu 2+ :CASM and Eu 2+ :CSASM show different behavior on the decay curves at low temperatures, satisfying t m n ( n >1). This discrepancy may be removed by several electron and/or hole centers with different trapping energy levels.     

TL, EPR and optical absorption in natural grossular crystal

Grossular is one of six members of silicate Garnet group. Two samples GI and GII have been investigated concerning their luminescence thermally stimulated (TL). EPR and optical absorption and the measurements were carried out to find out whether or not same point defects are responsible for all three properties. Although X-rays diffraction analysis has shown that both GI and GII have practically the same crystal structure of a standard grossular crystal, they presented different behavior in many aspects. The TL glow curve shape, TL response to radiation dose, the effect of annealing at high temperatures before irradiation, the dependence of UV bleaching parameters on peak temperature, all of them differ going from GI to GII. The EPR signals around g=2.0 as well as at g=4.3 and 6.0 have much larger intensity in GI than in GII. Very high temperature (>800 °C) annealing causes large increase in the bulk background absorption in GI, however, only very little in GII. In the cases of EPR and optical absorption, the difference in their behavior can be attributed to Fe³⁺ ions; however, in the TL case one cannot and the cause was not found as yet.     

Structural and photoluminescence properties of silicon nanocrystals embedded in SiC matrix prepared by magnetron sputtering

Si nanocrystals (NCs) embedded in an SiC matrix were prepared by the deposition of Si-rich Si_1?xC_x/SiC nanomultilayer films using magnetron sputtering, subsequently followed by thermal annealing in the range of 800～1200 °C. As the annealing temperature increases to 1000 °C, Si NCs begin to form and SiC NCs also start to emerge at the annealing temperature of 1200 °C. With the increase of annealing temperature, two photoluminescence (PL) peaks have an obvious redshift. The intensity of the low-energy PL peak around 669～742 nm gradually lowers, however the intensity of high-energy PL peak around 601～632 nm enhances. The low-energy PL peak might attribute to dangling bonds in amorphous Si (a-Si) sublayers, and the redshift of this peak might be related to the passivation of Si dangling bonds. Whereas the origin of the high-energy PL peak may be the emergence of Si NCs, the redshift of this peak correlates with the change in the size of Si NCs.     

KTN thin films prepared by pulsed laser deposition on transparent single crystal quartz(100)

Using the Sol-Gel method to produce the KTN ultrafine powder and the sintering technique with K2O atmosphere to prepare KTN ceramics as the targets instead of the KTN single crystal, highly oriented KTN thin films were produced on the transparent single crystal quartz (100) by the pulsed laser deposition (PLD). Since the thermal stress sustained by the quartz is relatively small, the limit temperature of the quartz substrates (300℃) is much lower than that of the P-Si substrates (560℃); the prepared thin film is at amorphous state. Increasing the pulsed laser energy density in the process incorporated with annealing the film after deposition at different temperatures converts the amorphous films into crystal. The optimal pulsed laser energy density and annealing temperature were 2.0 J/cm2 and 600℃, respectively. A discussion was made to understand the mechanism of film production at relatively low substrate temperature by PLD and effects of the annealing temperatures on the forming of the perovskite p     

Fabrication of nanopatterned sapphire substrates by annealing of patterned Al thin films by Laser Interference Lithography

Nanopatterned sapphire substrates were fabricated by annealing of patterned Al thin films. Square-patterned Al thin films with the diagonal length of 600 nm, period of 1 um and height of ～200 nm were obtained by the Laser Interference Lithography and Reactive Ion Etching. Patterned Al thin films were subsequently subjected to dual stage annealing due to the melting temperature of Al thin films (660 ^°C). The first comprised a low temperature oxidation anneal. The hillocks formation on Al thin films was minimized with an oxidation annealing at 450 ^°C for 24 h. The little change in the morphology of patterned Al thin films was observed at 450 ^°C for 24 h. This was followed by a high temperature annealing to induce growth of the underlying sapphire single crystal to consume the oxide layer. The SEM results show the patterns were retained on sapphire substrates after high temperature annealing at less than 1200 ^°C. The XRD and Raman results reveal that the orientation of island patterns by dual stage annealing of patterned Al thin films for 24 h at 450 ^°C, and 1 h at 1000 ^°C, was the same as that of the sapphire (0001) substrates.     

The millimeter-wave dielectric properties of Al2O3 after irradiation to moderate neutron fluence

Abstract

Mono- and polycrystalline Al₂O₃ has been irradiated to 3.5· 10¹⁹ f.n/cm², and the increase in dielectric loss has been measured at 28–38 GHz and 144–146 GHz. Step annealing experiments have been performed between 150 °C and 1100 °C. The recovery of dielectric loss has been analyzed aiming at identifying the defect types affecting dielectric loss. A pronounced recovery step observed at 450–550 °C is explained by F-centres with strong electron-lattice coupling which contribute predominantly to dielectric loss at room temperature.     

In-situ and ex-situ study of crystallization behaviour of magnetron sputtered Ni63Zr37 amorphous thin film

ABSTRACT

The stages of crystallization of magnetron sputter-deposited Ni₆₃Zr₃₇ film with mostly amorphous structure have been investigated by differential scanning calorimetry (DSC) and in-situ annealing at 300°C by use of heating stage on a high-resolution transmission electron microscope (HRTEM). These results have been further confirmed by grazing incidence X-ray diffraction analyses of thin film specimens annealed ex-situ at 300°C for various durations. The temperature for crystallization found by DSC has been found to increase from 371°C to 434°C with an increase in heating rate from 3°C/min to 10°C/min, and the apparent activation energy for amorphous to crystalline transformation has been found as ～260.2?kJ/mol from the Kissinger plot. Studies on HRTEM using in-situ heating stage have shown the crystallization to occur on annealing at 300°C for ～10?min. Crystallization at a temperature lower than that found by DSC is attributed to structural relaxation with reduction of free volume due to thermal activation. It has been observed that Ni₃Zr forms first due to its large negative enthalpy of formation, and is followed by the formation of Ni-rich solid solution (Ni_ss) grains. HRTEM studies have shown grain rotation with the formation of partial dislocations at Ni₃Zr-Ni_ss interfaces as well as twinning followed by detwinning with dislocation formation in the Ni_ss matrix possibly to reduce the interfacial energy.     

Hot electron studies of lattice damage created in silicon by implantation of 2.8 MeV protons

Abstract

In this paper we report the results of a study of the annealing properties of the ionized defect density associated with the damage created in the silicon lattice by implantation of 2.8 MeV protons at room temperature. In particular, the annealing of damage created by implanting to a level of 4.43 × 10¹² protons/cm² is reported. The resulting isochronal annealing curve covered the temperature range from 70°C to 460°C. Two major annealing stages are discussed, one a broad stage between 70°C to 200°C and the other an abrupt annealing stage between 440°C to 460°C. Between the temperature range 200°C to 440°C the number of ionized defects remained relatively constant. Above 460°C no detectable effects of the proton implantation remained.     

Laser annealing of radiation defects in low disordered layers

Abstract

Carrier concentration and mobility dependences on the annealing temperature have been compared for the cases of thermal (10 min) and laser (8 ms) annealing of silicon, implanted with low doses of P⁺ ions. It was found that the recovery of concentration and mobility depended on the heating time in different ways. The laser annealing requires higher temperatures for mobility recovery then the thermal treatment. The same temperature shift was observed for increase of carrier concentration but only after doses less than 3.10¹²m^?2. When the doses exceeded 3.10¹² cm^?2 laser and thermal annealing resulted in equal electron concentrations providing the equality of heating temperatures. Annealing of disordered regions was accounted for the mobility recovery. The increase of electron concentration was explained as an instantaneous decay of defect-impurity complexes. To check the validity of the assumptions laser annealing of electron and light ions irradiated materials was investigated.     

Correlation between microstructure and optical properties of nano-crystalline TiO2 thin films prepared by sol-gel dip coating

Titanium dioxide thin films have been prepared from tetrabutyl-orthotitanate solution and methanol as a solvent by sol-gel dip coating technique. TiO₂ thin films prepared using a sol-gel process have been analyzed for different annealing temperatures. Structural properties in terms of crystal structure were investigated by Raman spectroscopy. The surface morphology and composition of the films were investigated by atomic force microscopy (AFM). The optical transmittance and reflectance spectra of TiO₂ thin films deposited on silicon substrate were also determined. Spectroscopic ellipsometry study was used to determine the annealing temperature effect on the optical properties and the optical gap of the TiO₂ thin films. The results show that the TiO₂ thin films crystallize in anatase phase between 400 and 800 °C, and into the anatase-rutile phase at 1000 °C, and further into the rutile phase at 1200 °C. We have found that the films consist of titanium dioxide nano-crystals. The AFM surface morphology results indicate that the particle size increases from 5 to 41 nm by increasing the annealing temperature. The TiO₂ thin films have high transparency in the visible range. For annealing temperatures between 1000 and 1400 °C, the transmittance of the films was reduced significantly in the wavelength range of 300-800 nm due to the change of crystallite phase and composition in the films. We have demonstrated as well the decrease of the optical band gap with the increase of the annealing temperature.     

Defect states in Lu 3 Al 5 O 12 :Ce crystals

Wavelength-resolved TSL measurements after x-ray irradiation at room temperature were performed on undoped, Ce- and (Ce, Zr)-doped Lu 3 Al 5 O 12 crystals. Several glow peaks were observed in the 20-450 v C temperature region, whose intensities and emission spectra are influenced by doping. Namely, the TSL spectra are governed by defect and trace impurity-related emissions in the undoped crystal, while only the Ce 3+ emission is detected in the doped crystals. Moreover, EPR measurements performed at 12 v K revealed typical spectra of Ce 3+ (4f 1 , S =1/2) occupying Lu 3+ substitutional positions. In situ light irradiation (250-330 v nm) of the crystals results in a step-like decrease of the Ce 3+ EPR intensity. Such a behaviour can reflect a creation of Ce 4+ ions under UV irradiation or an increase of the Ce 3+ population in the excited (5d) state.     

Discovery of a self-trapped-electron center in α-TeO 2

Electron spin resonance (ESR) studies show that electron irradiation of an f -TeO 2 single crystal followed by 330-nm UV illumination at ～10 v K generates a new spin-1/2 paramagnetic center having C 2 symmetry, like the Te lattice sites, that is attributed to a self-trapped charge on a Te. Identification is facilitated by a strong hyperfine interaction with 125 Te at a central Te site and weaker 125 Te superhyperfine interactions with three different equivalent pairs of neighboring Te cations. The irradiations also produce the diamagnetic V_{O}^{\times} center and the paramagnetic V_{O}^{\bullet} and V_{O}^{\prime} centers. From measurements of concentration changes of the paramagnetic centers due to thermal annealing of the new center it is deduced that the self-trapped charge is a self-trapped electron. It is designated as a \hbox{TeO}_{2}^{\prime} center. This assignment is consistent with its low thermal stability since it anneals quickly at temperatures above 40 v K. ESR characteristics of this new center are described.     

Effects of Annealing Temperature on Structural and Optical Properties of ZnO Thin Films

The effects of annealing temperature on the structural and optical properties of ZnO films grown on Si （100） substrates by sol-gel spin-coating are investigated. The structural and optical properties are characterized by x-ray diffraction, scanning electron microscopy and photoluminescence spectra. X-ray diffraction analysis shows the crystal quality of ZnO films becomes better after annealing at high temperature. The grain size increases with the temperature increasing. It is found that the tensile stress in the plane of ZnO films first increases and then decreases with the annealing temperature increasing, reaching the maximum value of 1.8 GPa at 700℃. PL spectra of ZnO films annealed at various temperatures consists of a near band edge emission around 380 nm and visible emissions due to the electronic defects, which are related to deep level emissions, such as oxide antisite （OZn）, interstitial oxygen （Oi）, interstitial zinc （Zni） and zinc vacancy （VZn^-）, which are generated during annealing process. The evolution of defects is analyzed by PL spectra based on the energy of the electronic transitions.     

Effects of annealing temperature on the alloying behavior of the AuGe-GaAs〈100〉 interface

UV(He I) and X-ray photoelectron spectroscopies (UPS and XPS) were used to examine the alloying behavior of AuGe ohmic contacts to silicon-doped 100 oriented n-type GaAs substrates. The reacted interface was then revealed by Ar ion sputter depth profiling at room temperature and after annealing in ultra high vacuum at 300°, 500°, or 700°C. The indiffusion of Au and the outdiffusion of Ga and As are evident. Instead of obtaining a maximum peak of the Ge profile on annealing in forming gas, we observed an increase of Ge indiffusion with temperature. The Au indiffusion results in a decrease in the Au 5d splitting and a shift of both levels to higher binding energy. Au-Ga alloy formation is indicated by the Au 4f levels, and is further supported by the observation of the metallic Ga peak. It has been concluded that the sample annealed at 500°C forms the Au-Ga alloy and the compound of As containing Ge more easily than the samples annealed at 300° or 700°C. This result is consistent with the observations of low contact resistance at the annealing temperature of 500°C for AuNiGe ohmic contacts to n-type GaAs.     

Recrystallization of pure and strontium-doped KCl crystals

The kinetics of microstructure transformations are studied during annealing of deformed single crystals of KCl and KCl:0.05wt %Sr²⁺ at temperatures of (0.35–0.55)T _m (where T _m is the melting temperature) and during storage at room temperature. The effect of deformation rates ranging from 0.01 mm/min to 0.1 mm/min at a deformation temperature T _d=0.5T _m on the crystal structure and on the recrystallization kinetics is noted. It is found experimentally that the incubation period for static recrystallization in single-crystal KCl:0.05wt%Sr²⁺ is shortened and recrystallization takes place at room temperature after deformation in this temperature range. Here, during the new recrystallization grains have a twinned orientation with respect to the initial single crystal during the first stage and to the subgrains of the deformed crystal. As the annealing temperature is raised, the stage in which twins grow in KCl:0.05wt%Sr²⁺ crystals is shortened and it is displaced by recrystallization through migration of high-angle grain boundaries of the common type. Deformation conditions which ensure prolonged (at least three months) stability of the post-deformation hardening of single crystals are found experimentally for Sr²⁺-doped deformed single crystals. Fiz. Tverd. Tela (St. Petersburg) 41, 259–264 (February 1999)     

Investigation of defect structures in deuteron irradiated and deformed stainless steel 316 by positron annihilation

Abstract

Deuteron-irradiated and deformed stainless steel specimens were investigated by positron lifetime and Doppler broadening measurements. The evolution of the defect structures was studied as a function of the isochronal annealing temperature and for various degrees of deformation. A different behaviour was observed for deformed and irradiated stainless steel specimens. Evidence for vacancy clusters was found in the deuteron-irradiated steel. These clusters disappear after annealing around 900 K.