Nanotomographic examinations of ion tracks in cellulose nitrate by ion energy loss spectrometry

Received: 13 October 1997/Accepted: 25 August 1998     

Fabrication of waveguides in Yb:YCOB crystal by MeV oxygen ion implantation

Oxygen ions with energies of 6.0 or 3.0 MeV were implanted into y-cut Yb:YCOB crystals at fluences ranging from 5.0 × 10¹³ to 2.0 × 10¹⁵ ions/cm² at room temperature, forming optical planar waveguide structures. Dark-mode line spectroscopy was applied at two wavelengths, 633 and 1539 nm, in various excitation configurations, showing strong enhancement of one of the indices (n_x) in the implanted near surface. The n_x refractive index profile is reconstructed by a reflectivity calculation method and compared to the ion energy losses profiles deduced from SRIM-code simulation. Moreover, the near-field patterns were imaged by an end-fire coupling arrangement.     

Reflectivity modification of polymethylmethacrylate by silicon ion implantation

The effect of silicon ion implantation on the optical reflection of bulk polymethylmethacrylate (PMMA) was examined in the visible and near UV. A low-energy (30 and 50 keV) Si⁺ beam at fluences in the range from 10¹³ to 10¹⁷ cm⁻² was used for ion implantation of PMMA. The results show that a significant enhancement of the reflectivity from Si⁺-implanted PMMA occurs at appropriate implantation energy and fluence. The structural modifications of PMMA by the silicon ion implantation were characterized by means of photoluminescence and Raman spectroscopy. Formation of hydrogenated amorphous carbon (HAC) layer beneath the surface of the samples was established and the corresponding HAC domain size was estimated.     

Positron and deuteron depth profiling in helium-3-implanted electrum-like alloy

In spite of previous extensive studies, the helium behavior in metals still remains an issue in microelectronics as well as in nuclear technology. A gold-silver solid solution (Au₆₀Ag₄₀: synthetic gold-rich electrum) was chosen as a relevant model to study helium irradiation of heavy metals. After helium-3 ion implantation at an energy ranging from 4.2 to 5.6 MeV, nuclear reaction analysis (NRA) based on the ³He(d,p)⁴He reaction, was performed in order to study the thermal diffusion of helium atoms. At room temperature, NRA data reveal that a single Gaussian can fit the He-distribution, which remains unchanged after annealing at temperatures below 0.45 of the melting point. Slow positron implantation spectroscopy, used to monitor the fluence dependence of induced defects unveils a positron saturation trapping, which occurs for He contents of the order of 50-100 appm, whereas concentrations larger than 500 appm seem to favor an increase in the S-parameter of Doppler broadening. Moreover, at high temperature, NRA results clearly show that helium long range diffusion occurs, though, without following a simple Fick law.     

Ion implantation inducing nanovoids characterized by TEM and STEM

The evolution of nanoparticles in sequentially ion-implanted Ag and Ag/Cu into silica glasses has been studied. The doses for implantation (×10¹⁶ ions/cm²) were 5Ag, 5Ag/5Cu and 5Ag/15Cu. Ag nanoclusters have been formed in the implanted 5Ag specimen. In the implanted 5Ag/5Cu specimen, some formed nanoclusters have brighter center features. With an increase of Cu ions dose, the nanoclusters with brighter center features become prevalent. The microstructural properties of the nanoparticles are characterized by transmission electron microscopy. Scanning transmission electron microscope high-angle annular dark field and high-resolution transmission electron microscopy are also utilized to study the formed nanoparticles. The results show that nanovoids have been induced into metal nanoparticles during the ion implanting process, not the core-shell nanoparticles as other workers believed. The nanovoids can be the aggregation of vacancies induced by irradiation.     

Characterization of optical waveguide in Nd: GdVO4 by triple-energy oxygen ion implantation

We report on the optical planar waveguide formation and modal characterization in Nd: GdVO₄ crystals by triple oxygen ion implantation at energies of (2.4, 3.0, and 3.6 MeV) and fluences of (1.4, 1.4, and 3.1)  × 10¹⁴ions/cm². The prism-coupling method is used to investigate the dark-mode property at wavelength of 632.8 nm. The refractive index profiles of the waveguide are reconstructed by an effective refractive index, n_eff method. The modal analysis shows that the fields of TE modes are well restricted in the guiding region, which means the formation of nonleaky waveguide in the crystal.     

Surface Disorder of GaN Irradiated by Highly Charged Arq+-Ions

The surface damage to gallium nitride films irradiated by Ar^q＋ （6≤q≤16） ions at room temperature is studied by the atomic force microscopy. It is found that when charge state exceeds a threshold value, significant swelling was turned into obvious erosion in the irradiated region. The surface change of the irradiated region strongly depends on the charge state and ion fluence. On the other hand, surface change is less dependent on the kinetic energy nearly in the present experimental range （120 keV≤Ek≤220 keV）. For q≤14, surface of the irradiated region is covered with an amorphous layer, rough and bulgy. A step-up appears between the irradiated and un-irradiated region. Moreover, the step height and the surface roughness are functions of the ion dose and charge state, and increase with the increase of dose and charge state. Especially at and near boundary, a sharp bump like ridges in irradiated areas is observed, and there appear characteristic grooves in un-irradiated areas. For q=16, surface of the irradiated region was etched and erased.     

Characterization of optical waveguide in Nd: LuVO4 crystals by triple-energy oxygen ion implantation

We report on the optical planar waveguide formation and modal characterization in Nd:LuVO₄ crystals by triple-energy O³⁺-ion implantation at energies of 2.4, 3.0, and 3.6 MeV and doses of 1.4, 1.4, and 3.1×10¹⁴ ions/cm², respectively. The prism-coupling method is used to investigate the dark-mode property at a wavelength of 633 nm. The refractive index profiles of the waveguide are reconstructed by the reflectivity calculation method (RCM). The modal analysis shows that the fields of TE modes are well restricted in the guiding region, which indicates the formation of non-leaky waveguide in the crystal.     

Nonlinear optical properties of Cu nanoclusters by ion implantation in silicate glass

Metal nanocluster composite glass prepared by 180 keV Cu ions into silica with dose of 1 × 10¹⁷ ions/cm² has been studied. The microstructural properties of the nanoclusters were analysed by optical absorption spectra and transmission electron microscopy (TEM). Third-order nonlinear optical properties of the nanoclusters were measured at 1064 nm and 532 nm excitations using Z-scan technique. The nonlinear refraction index, nonlinear absorption coefficient, and the real and imaginary parts of the third-order nonlinear susceptibility were deduced. The mechanisms responsible for the nonlinear response were discussed. Absolute third-order nonlinear susceptibility χ⁽³⁾ of this kind of sample was determined to be 2.1 × 10⁻⁷ esu at 532 nm and 1.2 × 10⁻⁷ esu at 1064 nm, respectively.     

Characterization of laser waveguides in Nd:CNGG crystals formed by low fluence carbon ion implantation

We report on Nd:CNGG active planar waveguides produced by 6.0 MeV carbon ion implantation at fluence from 1 × 10¹⁴ ions/cm² to 8 × 10¹⁴ ions/cm². The refractive index profiles, which were reconstructed according to the measured dark mode spectroscopy, showed that the refractive indices had negative changes in the surface region, forming typical barrier waveguide. The width of waveguide structure induced by carbon ion implantation is ∼3.8 μm. The typical barrier-shaped distribution may be mainly due to the nuclear energy deposition of the incident ions into the substrate. By performing a modal analysis on the observed TE modes, it was found that the TE₀ and TE₁ modes can be well-confined inside the waveguide.     

Surface Erosion of GaN Bombarded by Highly Charged 208Pbq+-Ions

Surface change of gallium nitride specimens after bombardment by highly charged Pbq^＋-ions （q = 25, 35） at room temperature is studied by means of atomic force microscopy. The experimental results reveal that the surface of GaN specimens is significantly etched and erased. An unambiguous step-up is observed. The erosion depth not only strongly depends on the charge state of ions, but also is related to the incident angle of Pbq^＋-ions and the ion dose. The erosion depth of the specimens in 60° incidence （tilted incidence） is significantly deeper than that of the normal incidence. The erosion behaviour of specimens has little dependence on the kinetic energy of ion （Ek = 360, 700 keV）. On the other hand, surface roughness of the irradiated area is obviously decreased due to erosion compared with the un-irradiated area. A fiat terrace is formed.     

Fabrication of ferromagnetic (Ga,Mn)As by ion irradiation

Using Mn⁺ implantation following ion beam-induced epitaxial crystallization (IBIEC) annealing, high Curie temperature ferromagnetic (Ga,Mn)As thin film was fabricated. The crystalline quality of the Mn⁺ implanted layer was identified by X-ray diffraction (XRD) and transmission electron microscopy (TEM). A clear ferromagnetic transition at T_c 253 K was observed by magnetization vs. temperature measurement. We infer that IBIEC treatment is a useful method not only for the low-temperature annealing of (Ga,Mn)As thin films but also for other dilute magnetic semiconductor (DMS) samples.     

Tomographic study of the three-dimensional distribution of a high-fluence implant in a polymer

6 Li⁺ ions were implanted into PMMA at high flux up to fluences of 1×10¹⁵ cm^-2 under angles of 0° to 70° towards the surface normal. The Li depth distributions were determined by means of neutron depth profiling, and compared with theoretical simulations. The three-dimensional Li distribution was reconstructed from the one-dimensional depth profiles by means of a tomographic technique. It turned out that the measured Li depth distributions can be described by a superposition of Gaussian and exponential functions. This points at considerable Li mobility during or after the ion implantation, with trapping in unsaturable traps in the ion-irradiated region which roughly follow the electronic energy transfer distribution. The Li redistribution is more pronounced along the track direction than transversely to it. The normalized Li distributions in various implantation directions were fed into our tomographic program to reconstruct the three-dimensional distribution of the deposited lithium. As expected, the lithium preferentially distributes along the ion tracks. This work is another hint that mobility of implanted ions in solids does not proceed isotropically, but is strongly influenced by the radiation-damage distributions. Received: 11 May 1998 / Accepted: 9 September 1998 / Published online: 24 February 1999     

The characterization of mechanical and surface properties of poly (glycerol-sebacate-lactic acid) during degradation in phosphate buffered saline

The present study synthesized a poly (glycerol-sebacate-lactic acid) (PGSL) with 1:1:0.5 mole ratio of glycerol, sebacate and lactic acid and investigated the degradation characteristics of the polymer in phosphate buffered saline (PBS) at 37 °C in vitro by means of mass loss tests, geometry, differential scanning calorimeter (DSC) measurements, tensile analysis and scanning electron microscopy (SEM). The maintained geometry, linear mass loss, and minor crack formation on the surface during degradation characterized both the bulk degradation and surface erosion of the polymer. By day 30 of degradation, the mass lost reached 16%. The elastic modulus, tensile strength and elongation at breakage of PGSL were correlative to the period of degradation.     

Improved optical response and photocatalysis for N-doped titanium oxide (TiO2) films prepared by oxidation of TiN

In order to improve the photocatalytic activity, N-doped titanium oxide (TiO₂) films were obtained by thermal oxidation of TiN films, which were prepared on Ti substrates by ion beam assisted deposition (IBAD). The dominating rutile TiO₂ phase was found in films after thermal oxidation. According to the results of X-ray photoelectron spectroscopy (XPS), the residual N atoms occupied O-atom sites in TiO₂ lattice to form TiON bonds. UV-vis spectra revealed the N-doped TiO₂ film had a red shift of absorption edge. The maximum red shift was assigned to the sample annealed at 750 °C, with an onset wavelength at 600 nm. The onset wavelength corresponded to the photon energy of 2.05 eV, which was nearly 1.0 eV below the band gap of pure rutile TiO₂. The effect of nitrogen was responsible for the enhancement of photoactivity of N-doped TiO₂ films in the range of visible light.     

Formation of Cu nanoparticles in GaAs using MeV ion implantation followed by thermal annealing

Analytical electron microscopy, high-resolution X-ray diffraction and combined Rutherford backscattering spectrometry and channeling experiments have been used to investigate the radiation damage and the effect of post-implantation annealing on the microstructure of GaAs(100) single crystals implanted with 1.00 MeV Cu⁺ ions to a dose of ≈ 3×10¹⁶ cm^-2 at room temperature. The experiments reveal the formation of a thick and continuous amorphous layer in the as-implanted state. Annealing up to 600 °C for 60 min does not result in the complete recovery of the lattice order. The residual disorder in GaAs has been found to be mostly microtwins and stacking fault bundles. The redistribution of implanted atoms during annealing results in the formation of nano-sized Cu particles in the GaAs matrix. The X-ray diffraction result shows a cube-on-cube orientation of the Cu particles with the GaAs lattice. The depth distribution and size of the Cu particles have been determined from the experimental data. A tentative explanation for these results is presented. Received: 15 February 1999 / Accepted: 18 February 1999 / Published online: 28 April 1999     

Kinetics of reversible surface crystallization and melting in poly(ethylene oxide): Effect of crystal thickness observed in the dynamic heat capacity

Poly(ethylene oxide) (PEO) in the semi-crystalline state shows a reversible surface crystallization and melting; a temperature decrease leads to a certain crystal thickening, a temperature increase reversely to an expansion of the amorphous intercrystallite layers. Dynamic calorimetry provides a means to investigate the kinetics of the process. The structural rearrangement in the region of the crystalline-amorphous interface can only be accomplished if the chains can slide through the crystallites. One therefore expects the associated time to change with the crystallite thickness. Variations of the crystal thickness of PEO can be achieved by choosing different crystallization temperatures. We studied the effect of the crystal thickness employing temperature-modulated differential scanning calorimetry and heat wave spectroscopy, and by carrying out small-angle X-ray scattering experiments for the structural characterization. The effect of the crystal thickness is clearly observed. Results indicate that the sliding diffusion through the crystallites takes place by helical jumps of whole stems. Data yield the activation energy per unit length of the stems. Received 20 April 2001 and Received in final form 13 August 2001     

Passivation of laser induced defects in silicon by low energy hydrogen ion implantation

It is well established that the pulsed-laser annealing of as-implanted Si introduces electrically active defects. The aim of this paper is to show that these defects can be neutralized by low-energy hydrogen ion implantation. The techniques used for the sample characterization are current-voltage measurements and capacitance transient spectroscopy.     

The optical properties of planar waveguides in LiB3O5 crystals formed by Cu implantation

A planar optical waveguide has been formed in a LiB₃O₅ crystal using 6.0 MeV Cu⁺-ions with a dose of 1 × 10¹⁵ ions/cm² at room temperature. Possible propagating modes were measured at a wavelength of 633 nm using the prism-coupling method. The refractive index profiles of the waveguide were reconstructed by an effective refractive index method and the beam propagation method was used to investigate the properties of the propagation modes in the formed waveguide. The results suggest that the fundamental TE₀ and TM₀ modes may be well-confined and propagate a longer distance inside the waveguide. The implantation process was also simulated using the transport of ions in matter code (TRIM), which indicates that the nuclear energy deposition may be the main factor for the refractive index change.     

Electrically conducting ion tracks in diamond-like carbon films for field emission

Electrically conducting channels in an insulating carbon matrix were produced by 140-MeV Xe ion irradiation. The high local energy deposition of the individual ions along their pathes causes a rearrangement of the carbon atoms and leads to a transformation of the insulating, diamond-like (sp³-bonding) form of carbon into the conducting, graphitic (sp²-bonding) configuration. The conducting ion tracks are clearly seen in the current mapping performed with an atomic force microscope (AFM). These conducting tracks are of possible use in field emission applications. Received: 4 May 1999 / Accepted: 5 May 1999 / Published online: 1 July 1999