Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2006

In-rich InGaN films (XIn>0.5) and InN/InGaN multi-quantum wells were grown on Ga- and N-polarity GaN templates by radio-frequency plasma-assisted molecular beam epitaxy. The In-polarity InGaN films grown at 450°C showed superior crystalline quality and smoother surface morphology compared to the N-polarity samples, which were grown at 500∼550°C. By using the In-polarity In0.7Ga0.3N as a barrier layer, the InN/InGaN multi-quantum wells were successfully fabricated on the III-element polarity GaN templates at 450°C. Fine periodic structures and strong photoluminescence emission around optical communication wavelength were obtained from the In-polarity MQWs. These results indicate that the In-polarity growth is preferred to obtain a high quality InGaN film and the InN/InGaN MQWs in spite of its lower growth temperature.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

We have grown InN quantum dots (QDs) on nitrogen-polarity (N-polarity) GaN under-layer by the radio-frequency plasma-assisted molecular beam epitaxy (RF-MBE), and systematically investigated growth mechanism of the InN dots. The InN QDs with the N-polarity could be grown at about 500°C, which was much higher than that of previous reports on InN dots grown by MBE. When the nominal coverage of InN became more than 1 mono-layer (ML), lattice relaxation of InN occurred and high density InN dots were uniformly formed. These results indicated that InN dots were formed by Stranski-Krastanov (S-K) growth mode. For the InN deposition above about 8ML, InN dots tended to coalesce and resulted in remarakable decrease of the dots density.

Epitaxy of InN films with N-polarity and In-polarity was investigated by RF-MBE with several in-situ monitoring/controlling systems. It was found that the epitaxy temperature for N-polarity growth could be as high as 600 °C and this was about 100 deg higher than that for In-polarity case. This temperature difference in two polarities drastically affected not only the growth behaviors but also the properties of InN epilayers, i.e. N-polarity growth was preferable in both view-points. The step-flow-like surface morphology was achieved for the InN films grown with N-polarity at 580 °C. The FWHMs of X-ray rocking curves for InN (002) and (102) of 5–8 μm-thick InN films grown in N-polarity were about 200–350 and 650–950 arcsec, respectively. The highest Hall mobility was above 2000 cm2/V·s with a background carrier concentration of 1–2×1018 cm−3 at room temperature. For both polarity films, N-rich condition was necessary for the stable InN growth to obtain 5–8 μm-thick InN films.

InN epitaxial layers are grown on sapphire substrates. The investigated samples have electron concentration in a range of 1.8 ×1018 − 1.1 ×1019 cm-3. Optical reflection and transmission measurements are performed. The plasma edge energy position in the spectra is constant in a measurement temperature range of 5 – 300 K. The reflection and transmission spectra are calculated on the basis of the LO phonon-electron coupling scheme and non-parabolic conduction band structure. From this analysis we find that the observed absorption edge is attributed to valence band to conduction band transition rather than the valence band to defect (impurity) band transition, and the intrinsic bandgap energy of 0.64 (±0.03) eV. This bandgap energy increases by 40 – 50 meV as the temperature decreases from 295 to 10 K.

In this study, we discuss a method for cross-sectional thin specimen preparation from a specific site using a combination of a focused ion beam (FIB) system and an intermediate voltage transmission electron microscope (TEM). A FIB-TEM compatible specimen holder was newly developed for the method. The thinning of the specimen using the FIB system and the observation of inside structure of the ion milled area in a TEM to localize a specific site were alternately carried out. The TEM fitted with both scanning transmitted electron detector and secondary electron detector enabled us to localize the specific site in a halfway milled specimen with the positional accuracy of better than 0.1 µm. The method was applied to the characterization of a precipitate in a steel. A submicron large precipitate was thinned exactly at its center for the characterization by a high-resolution electron microscopy and an elemental mapping.

A new method for transmission electron microscope (TEM) specimen preparation using a focused ion beam (FIB) system that results in a lower rate of gallium (Ga) implantation has been developed. The method was applied to structural and analytical studies of composite materials such as silicon (Si)-devices and magneto-optical disk. To protect the specimens against Ga ion irradiation, amorphous tungsten (W) was deposited on the surface of the specimen prior to FIB milling. The deposition was quite effective in reducing the Ga implantation rate, and energy-dispersive X-ray (EDX) analysis of these specimens detected 0.3Ð1.5% Ga incorporated in the thinned area. FIB milling times for these specimens were 1.5Ð2 hr. Although the milling rate was high, all the materials were properly prepared for TEM study, and clear crystal lattice images were observed on all specimens.

The structure and density of amorphous S1O2 films grown by chemical vapor deposition (CVD) or thermal oxidation are studied by Fourier-transform infrared (FT-IR) absorption, neutron diffraction, and Rutherford backscattering (RBS) measurements. CVD oxides, formed in an atmospheric-pressure CVD reactor with a SiH4-O2 gas mixture at 400 °C, are compared with thermal oxides, grown at 980 °C in H2-O2 atmosphere. The average Si-O-Si bond angle deduced from the stretching frequency of FT-IR is found to be smaller in CVD oxides than in thermal oxides, and the density revealed by RBS measurements is found to be a little lower in CVD oxides than in thermal oxides. These differences are explained by the medium-range structural disorder revealed by FT-IR measurements as well as by neutron diffraction measurements. The medium-range structural disorder in CVD oxides is responsible for large silanol content in the oxides and is the origin in difference between CVD and thermal oxides.

SrTiO3 thin films were prepared by ECR and thermal MOCVD. In thermal-CVD mode, Sr content and Ti content were at a maximum at 0.56 Torr. Results showed that SrO deposition is a surface reaction limited process between 500 and 650°C, whereas TiO2 deposition is surface reaction limited between 500 and 600 °C, and diffusion limited above 600 °C. At a low pressure of 8 mTorr, ECR oxygen plasma was found to help decompose Ti(i-OC3H7)4. In ECR-CVD mode, the deposition temperature could be lowered to 400 °C. TEM and SEM analyses showed that SrTiO3 thin films have a columnar structure. The size of the grains depends on film thickness, and their shape on film composition (Sr/Ti ). Films prepared by thermal-CVD had a lateral step coverage of 50 %. 40 nm SrTiO3 thin films (Sr/Ti = 1.0) prepared by thermal-CVD on Pt/TaOx/Si and annealed for 2 hours in O2 had a maximum dielectric constant of 139 (Cs = 31 fF/μm2 and teq = 1.1 nm) and a leakage current density of 6x10−8 A/cm2 at 1.0 V.

30-keV focused Ga+ ion beam was used for induced deposition of small-area tungsten thin films from W(CO)6 on Si and SiO2. Deposition yield, calculated assuming pure tungsten depositions, depends on dwell time (beam diameter/scan speed) and beam current density. High current density and/or long dwell time are known to cause low deposition yield because of the depletion of adsorbed gas molecules during ion beam irradiation. Based on a model taking this effect into account, numerical fitting was carried out. The reaction cross-section was estimated to be 1.4 × 10−14 cm2. For doses below 1017 ions/cm2, film resistivity decreases with increasing dose. This was confirmed for several dwell times. However, for doses above 1017 ions/cm2, film resistivity remains independent of dose. In this “high”-dose range, variation of beam current density has little effect on film resistivity. AES analyses revealed a consistency between film composition and resistivity. For a “high”-dose film with a resistivity of 190 μΩ-cm, the approximate tungsten content was 50 at%.

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.

Silicon vapor phase epitaxial growth with SiH2Cl2 is theoretically studied. The optimized geometries and total energigs of the species, generated from SiH2Cl2, are calculated by using ab initio molecular orbital method. As the intgraction between silicon surface and SiCl2 the charge transfer is considered. Based on the computational result that SiCl2 - has the lower total energy than SiCl2, a new adsorption mechanism, named, charge transfer adsorption, is p~oposed. By using this charge transfer adsorption followed by the surface reaction at the hollow bridge site, the epitaxial growths on the silicon (001), (111), and (110) surfaces are discussed.

The stress induced transformation in Y2 O3 containing tetra gonal zirconia polycrystals (Y-TZP) by a three-point bending test was studied by Raman microprobe. Transformation zone extends to as large as 100μm in the starting side of the fracture and the transformation zone size becomes smaller in the direction from the starting to the ending side of the fracture. The transformation zone size has no correlation with fracture toughness and Y2O3 content. It is suggested that the transformation plastici y may operate in the initial stage of the fracture. The obtained results have remarkable contrast with the case of the fracture of a pre-indented specimen. The transformation behavior of defect-dominating fracture is also discussed.