Three-dimensional (3D) observation is one of the important trials of future TEM and STEM methods. in the field of biological science, 3D-observation has already become general because the biological materials are usually amorphous and computed tomography (CT) routines can be effectively used. The CT assumes that the image intensity is linearly proportional to the projection of material density. in a crystalline specimen, however, this linearity does not hold due to the dynamical diffraction effect depending on spepimen thickness and incident directions of electron beam. High-angle annular-darkfield STEM (HAADF-STEM) and EDX mapping images could meet this requirement of the linearity because their image intensity are little affected by the dynamical diffraction effect.

Our 3D-STEM is based on a 300 kV FE-TEM/STEM(Hitachi HF-3000) equipped with a specially designed eucentric specimen stage with double spherical fulcra, a newly developed dark/bright field STEM detectors, a 3D-sampling system and a 3D-imaging processor for 3D topography and tomography.

The relationship among electrical conductivity, optical properties, and carbon structure of ion-implanted polymers has been studied by optical transmission and Raman spectroscopy. The electrical conductivity, which depends not only on the ion dose but also on the dose rate in a complicated manner, was found to have a simple relation to the optical absorbance. By Raman spectroscopic analyses, the difference in the electrical conductivity was explained in terms of the difference in carbon structure.

The electrochemical properties of O+-implanted Pd measured by cyclic voltammetry in a 0.25 mol dm-3 H2SO4 solution were investigated in relation to their composition and structure. Implantation of 16O+ was performed with doses between 1O17 and 1O18 ions cm-2 at 150 keV, and at nearly room temperature. SIMS, ERD combined with RBS, and XRD were used to analyze the composition depth profile and structure of O+-implanted Pd surface layers. The H atoms were accumulated with a gaussian distribution and carbon materials containing the solid solution of PdCx (x=0.13-0.15) were also formed in the near surface layers during O+-implantation. The distribution of implanted oxygen changed from gaussian to trapezoidal as the dose increased, accompanied by the crystal growth of Pd(OH)2, and simultaneously, the amount of accumulated H atoms increased. The voltammetric measurements revealed that with an increase in the dose, the hydrogen absorption was suppressed at the early stage of sweep cycles, and at the final stage, the redox reaction of both hydrogen and Pd was activated. From these results, we propose that the carbon materials containing the PdCx formed during O+-implantation suppress the hydrogen absorption, and the metallic Pd like a Pd-black formed by the reduction of Pd(OH)2 during voltammetric measurements causes the electrochemical activation of O+-implanted Pd.

A study has been made of the carbon formation in the surface layer of Ag-, W- and Pd-ions implanted polyimide films. The doses of 130 KeV Ag-ions and 190 KeV W-ions ranged from lxlO16 to 5×1017 atoms/cm2. The doses of 100 KeV Pd-ions ranged from 5×1016 to 2×1017 atoms/cm2. The carbon structure in implanted layers was characterized by laser Raman spectroscopy (LRS). Non-implanted polyimide film has very strong intensity of fluorescence, and the intensity of all W-, Ag- and Pd-ions implanted specimens decreases with the increase in dose. The intensity of Raman spectra for both W- and Ag-ions implanted specimens increases with the increase in dose. For Pd-ion implanted specimens, the Raman spectrum of carbon is hardly observed even with a high dose. Raman spectra for W- or Ag-ions implanted specimens with a high dose show that the diamond-like carbon (DLC) exist in the implanted layers. It is found that the DLC structures in the W- and Ag-ions implanted layers have graphite-like and amorphous-like structures, respectively. We propose that transparency carbon structure in implanted layers is generated by Pd-ion implantation. It is concluded that marked DLC formation in surface layer of polyimide films can be caused by Ag- or W-ions implantation except Pd-ion implantation, and carbon structure in implanted layers depends strongly on the implanted elements.

A study has been made of the luminescence during Tb-ion implantation in Al2O3 or by Ar- or He-ions bombardment to Tb-ion implanted Al2O3. The substrates used were colorless and transparent single crystal ɑ-Al2O3 with (0001) or (1102) surface orientation. Ion implantations of Tb-ions in Al2O3 were carried out at fluences of 1x1013 to 1x1017 Tb/cm2 at 100 keV at nearly room temperature. Change in color of Al2O3, substrates by Tb implantation was invisible to the naked eye. The luminescence spectra were measured by Ar (100 keV) or He (50 keV) bombardment to Tb implanted Al2O3 or during Tb implantation into Al2O3 using a spectroscopy with three optical filters and photomultiplier. The luminescence spectra during Tb implantation into AljOj have four clear peaks identified as emission due to D-F transitions of Tb3+ state. The luminescence spectra of Tb implanted A12O3 excited by He, Ar and Tb bombardment were almost the same except for the luminescence at the wavelength ranging from 300 to 450 nm, which is caused by strong emission from A12O3 itself. The peak of the luminescence appears at 550 nm, and its intensity depends on the Tb dose. The maximum intensity of luminescence during Tb implantation at room temperature is obtained as the maximum atomic ratio of implanted Tb is 2–3 atomic %.

Ion implantation in silicone rubber has been carried out in order to study its effects on structure and chemical states. H+-, He+-, C+-, N+-, N2+-, O+-, O2+-, Ne+-, Na+-, Ar+-, and K+- ion implantations were performed at an energy of 150 keV with doses ranging from 1×1013 to 1×1017 ions/cm2 at room temperature. The depth profiles of the ion implanted elements and host elements were investigated by means of XPS and SIMS. The chemical properties were studied by FT-IR-ATR and Raman spectroscopy. XPS results indicated that most of the implanted elements showed a Gaussian like distribution in the silicone polymer matrix, but implanted He+, Ne+, and Ar+ could not be detected. Results of FT-IR-ATR showed that ion implantation broke CH3 and Si-O bonds to form new radicals such as SiOH, >C=0, CH2 and SiHx and the effects varied depending on the implanted ion species. The Raman spectroscopy results showed that ion implanted silicone contained both sp3 and sp2 bonded carbon.

Nitrogen molecular ion implantations have been performed in niobium thin films to form B 1-NbN layers with an accelerating voltage of 150 kV up to a dose of 5 × 1017 N2+ ions/cm2 at room temperature. Measurements of superconducting transition temperature (Tc), Auger electron spectroscopy analyses (AES), and x-ray diffraction analyses (XRD) have been carried out as a function of nitrogen dose in order to characterize the implanted layer. It has been found that there are two regions in the dose dependence of Tc; in the low-dose case, Tc decreases from the initial value of 8 K to less than 4.2 K with increasing dose, and in case of the high dose (more than 2.5 × 1017 ions/cm2) it increases rapidly to 11 K and becomes independent of the implantation dose. The XRD patterns indicate the generation of lattice disorder at the low dose, the formation of Nb2N and ∊NbN at the intermediate dose, and the formation of δNbN (B 1 structure) at the high dose; the selective growth of δNbN occurs at the highest dose, in spite of the fact that thermodynamically Nb2N and ∊NbN are equilibrium phases at room temperature and they are formed at the intermediate dose. In conclusion, high-dose nitrogen implantation at room temperature causes the formation of δNbN to increase Tc.

A study has been made on surface mechanical properties of Ti+-implanted Fe-Cr alloys with various Cr concentrations. The implantation was performed in the dose range from 1 × 1016 to 3×1017 Ti+/cm2 at the energy of 150keV. As the Cr concentration becomes lower, the friction coefficient of implanted alloys decreases, although the increase in the surface hardness is not obvious. XPS spectra show that the implantation caused the invation of carbon to form Fe-Cr-Ti-C metastable alloys containing chromium and iron carbides. It is concluded that Ti +-implantation is useful for decrease in friction of Fe-Cr alloys with the lower Cr concentration.

A study has been made on friction and hardness of boron and nitrogen ion implanted Fe-Cr alloys. Ion implantation has been carried out with doses ranging from 5 wt% up to 20 wt% at energies of 50, 100 and 150 keV at room temperature. Reciprocal traces for friction coefficient measurements were performed by using a Bowden-Leben tester at a low speed without lubricant. Hardness was measured by using a micro-Vickers tester at a load of 2gf. Hardness of the specimen increases after the implantation with either of ion species. Friction measurements with reciprocal sliding show that a life-time of decreased friction coefficient depends on implanted ion species, Cr concentrations and acceleration energies. For B+- implantation, the lower the chromium contents are, the longer a decreased friction coefficient lasts. Meanwhile, the friction reduced by nitrogen implantation lasts longer for higher chromium content substrates. Dependence of friction coefficient on an acceleration energy is discussed for B+-implantation.

Effects of N-implantation on the composition depth profile, the chemical bonds and the optical transmittance of AlNx films have been investigated by means of Auger Electron Spectroscopy (AES), Fourier Transform Infrared (FT-IR) spectroscopy and visible transmission spectroscopy. AINx films were deposited on silicon (111) and commercial glass by an Activated Reactive Eyaporation (ARE) technique near room temperature. The 40 and 80 keV N+ -implantations were carried out at room temperature with doses ranging from 5×1016 to 5×1017 ions/cm2. The result of AES measurements revealed that the as-deposited AlNx film on Si consists of the AIN layer near the topsurface and the Al-rich layer near the interface. The concentration of nitrogen in the films increases as the N-dose increases up to 1×1017 ions/cm2. The N-implantation at a dose of 5×1017 ion/cm2 causes the interface between the film and the Si substrate to mix rather than increase the nitrogen concentration in the film. This higher dose implantation makes the FT-IR absorption peak corresponding to Al-N bonding become clear, and it makes the optical transmittance at a wavelength of 4400 Å go from 7% for as-deposited AINx film up to 70–90%. It is concluded that N-implantation into AlNx films causes the formation of AIN with a stoichiometric ratio to improve optical properties of the film.

A study has been made on friction and hardness of boron and nitrogen ion implanted Fe-Cr alloys. Ion implantation has been carried out with doses ranging from 5 wt% up to 20 wt% at energies of 50, 100 and 150 keY at room temperature. Reciprocal traces for friction coefficient measurements were performed by using a Bowden-Leben tester at a low speed without lubricant. Hardness was measured by using a micro-Vickers tester at a load of 2gf. Hardness of the specimen increases after the implantation with either of ion species. Friction measurements with reciprocal sliding show that a life-time of decreased friction coefficient depends on implanted ion species, Cr concentrations and acceleration energies. For B+- implantation, the lower the chromium contents are, the longer a decreased friction coefficient lasts. Meanwhile, the friction reduced by nitrogen implantation lasts longer for higher chromium content substrates. Dependence of friction coefficient on an acceleration energy is discussed for B+-implantation.

Wear properties of Li+, K+, C+, Cl+, and Ti+ implanted glassy carbons (GC) have been studied by wear tests using silicon carbide abrasive paper. It has been found that ion implantation is effective for improving wear resistance of GC. The measurements of Raman spectra revealed formation of an amorphous structure on the surface. Anomalous depth profiles with flat concentration distribution of Li and K atoms were observed by a secondary ion mass spectroscopy (SIMS). In conclusion. the formation of an amorphous structure seems to explain the improvement in wear resistance.

A study has been made of the relationship between crystal structure and hardness of N-implanted Fe-surface layers. The substrates used were polycrystalline Fe-sheets 1 mm thick with a purity of 99.9 %. The ion implantation of 14N+ was performed with doses ranging from 7.5×1016 to 1×1018 ions/cm2 at an energy of 100 keV. The substrate temperatures during implantation were kept at -40, 20, 100 and 200 °C. The crystal structure of N-implanted layers was identified by X-ray diffraction method (XRD). The near surface hardness was measured by a Knoop hardness tester. The XRD patterns revealed that the iron-nitride peculiar to each implantation condition was formed, and the iron-oxide was embedded in the nitrides in case of higher temperature implantation. N-implantation led to hardness increase, whose degree also depended on implantation conditions. The comparison between the structure and hardness of implanted layers indicated that, among the phases of iron-nitrides produced by 20 °C implantation, ε-phase is the hardest and the γ-Fe203 and γ'-Fe4N formed by 200 °C implantation are harder than the ε-phase nitrides. These results are discussed with respect to the surface composition estimated by Rutherford backscattering spectrometry (RBS) using 1.5 MeV 4He+-ions.

A study has been made on the surface wettability, atomic ratio, chemical structure, chemical bonding states and plasma protein adsorption of ion implanted silicone rubbers. C+-, N2+-, 02+-, Ar+- and Na+-ion implantations were performed at an energy of 150 keV at room temperature. The doses ranged from 1x1012 to 1x1017 ions/cm2. Ion implantation caused the surface roughness to increase by 1–5 times. Surface wettability was estimated by means of a sessile drop method using water. With increasing ion dose, the contact angle of water decreased from 98.9° to 48.5°. However, if the sample was in the air, the contact angle of water returned to its initial valve in time elapsed. The results of XPS measurements showed that implanted elements were incorporated in a gaussian like distribution and host elements were redistributed in the polymer matrix. No change of binding energies of 01s, CIS, Si2p and Si2p can be observed upon ion implantation. Results of FT-IR-ATR showed that C+-, N2+-, 02+-, and Ar+-ion implantation decomposed the original chemical bonds to form the new radicals. The amounts of new radicals are related to doses of implanted ions. In contrast, Na+-ion implantation hardly formed new radicals. The amount of albumin adsorbed onto 02+-, Ar+-, N2+-, and C+- ion implanted silicone is less than that on unimplanted specimens, but more fibrinogen is adsorbed. Na+-ion implantation produced an increase in the amount of adsorbed albumin as the dose increased. In summary, Na+ion implantation produces effects that are attributable to the additional implanted constituent in the surface of the silicone, and 02+-, N2+-, C+-, and Ar+-ion implantations primarily cause radiation effects on silicone rubber.