• Journal of the Mineralogical Society of Korea
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• v.17 no.4
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• pp.327-338
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• 2004

XRD studies on annealed Na-feldspar (Amelia albite) at $1100^{\circ}C$ showed rapid structural changes due to Si-Al disordering, which resulted in phase transformations from low albite to high albite by 4-days annealing test. TEM SAED analyses on the annealed samples revealed a trend of structural changes, but estimation of the structural state was difficult due to a large deviation of the SAED data. Optimum conditions of CBED analyses on albite was established by employing a cooling specimen holder, 120 kV of acceleration voltage, 37 Jim of condenser aperture size and 25 nm of spot size. A proper orientation showing distinct changes of HOLZ lines corresponding to the structure changes of albite turned out to be close to the [418] direction with $-1.2^{\circ}$ tilting, where the width of two HOLZ lines in low albite was opposite to those in high albite.

• Applied Microscopy
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• v.29 no.1
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• pp.75-81
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• 1999

Optimum conditions for making the Au and Al internal standards for TEM have been determined experimentally. The Au internal standard was produced by sputter coating at 9mA for 100 seconds in low vacuum $(\leq1\times10^{-3})$. The Al internal standard was produced by evaporation coating at 7kV for 10 minutes in high vacuum $(\leq1\times10^{-5})$. Measurements of the lattice parameters of andalusite and albite feldspars with this Au internal standard resulted in errors of (a) $ \leq1.2%$ in precion and $\leq0.3%$ in accuracy for andalusite: (b) $\leq0.5%$ in precision and $\leq1.1%$ in accuracy for albite feldspars. The most significant error occurred from the measuring processes of distances and angles of electron diffraction patterns. By employing systematic procedures of measurement with high precision devices, this lattice parameter determination method utilizing the internal standard should be a good alternative to the conventional powder XRD method or the sophisticated CBED method for special samples.

• Applied Microscopy
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• v.25 no.2
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• pp.73-79
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• 1995

The oxidation of silicon wafers is an essential step in the fabrication of semiconductor devices. It is known to induce degradation of electrical properties and lattice strain of Si substrate from thermal oxidation process due to charged interface and thermal expansion mismatch from thermally grown SiO, film. In this study, convergent beam electron diffraction technique is employed to directly measure the lattice strains in Si(100) and $4^{\circ}$ - off Si(100) substrates with thermally grown oxide layer at $1200^{\circ}C$ for three hours. The ratios of {773}-{973}/{773}-{953} Higher Order Laue Zone lines were used at [012] zone axis orientation. Lattice parameters of the Si substrate as a function of distance from the interface were determined from the computer simulation of diffraction patterns. Correction value for the accelerating voltage was 0.2kV for the kinematic simulation of the [012]. HOLZ patterns. The change in the lattice strain profile before and after removal of oxide films revealed the magnitudes of intrinsic strain and thermal strain components. It was shown that $4^{\circ}$ -off Si(100) had much lower intrinsic strain as surface steps provide effective sinks for the free Si atoms produced during thermal oxidation. Thermal strain in the Si substrate was in compression very close to the interface and high concentration of Si interstitials appeared to modify the thermal expansion coefficient of Si.

• Applied Microscopy
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• v.25 no.3
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• pp.99-107
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• 1995

The morphological changes of primary solid particles as a function of process time on hypereutectic Al-15.5wt%Si alloy during semi-solid state processing with a shear rate of $200s^{-1}$ are studied. In this alloy, it was observed that primary Si crystals are fragmented at the early stage of stirring and morphologies of primary Si crystals change from faceted to spherical during isothermal shearing for 60 minutes. To understand the role of Al dissolved in the primary Si crystal by shear stress at high temperature, lattice parameters of the primary Si crystals are determined as a variation of high order Laue zone(HOLZ) line positions measured from convergent beam electron diffraction(CBED) pattern. The lattice parameter of the primary Si crystal in the rheocast Al-15.5wt%Si alloy shows tensile strain of about 5 times greater than that of the gravity casting. Increase of the lattice parameter by rheocasting is due to the increased amount of Al dissolved in the primary Si crystal accelerated by shear stress at high temperature. The amounts of solute Al in the primary Si crystal are measured quantitatively by EPMA method to confirm the CBED analysis.