• Journal of the Microelectronics and Packaging Society
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• v.28 no.1
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• pp.39-46
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• 2021

The quantitative measurement of interfacial adhesion energy (Gc) of multilayer thin films for Cu interconnects was investigated using a double cantilever beam (DCB) and 4-point bending (4-PB) test. In the case of a sample with Ta diffusion barrier applied, all Gc values measured by the DCB and 4-PB tests were higher than 5 J/㎡, which is the minimum criterion for Cu/low-k integration without delamination. However, in the case of the Ta/Cu sample, measured Gc value of the DCB test was lower than 5 J/㎡. All Gc values measured by the 4-PB test were higher than those of the DCB test. Measured Gc values increase with increasing phase angle, that is, 4-PB test higher than DCB test due to increasing plastic energy dissipation and roughness-related shielding effects, which matches well interfacial fracture mechanics theory. As a result of the 4-PB test, Ta/Cu and Cu/Ta interfaces measured Gc values were higher than 5 J/㎡, suggesting that Ta is considered to be applicable as a diffusion barrier and a capping layer for Cu interconnects. The 4-PB test method is recommended for quantitative adhesion energy measurement of the Cu interconnect interface because the thermal stress due to the difference in coefficient of thermal expansion and the delamination due to chemical mechanical polishing have a large effect of the mixing mode including shear stress.

• The Journal of Korean Academy of Prosthodontics
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• v.61 no.3
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• pp.179-188
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• 2023

Purpose. The purpose of this study was to evaluate the effect of surface treatments on the shear bond strength of two types of zirconia (3-TZP and 5Y-PSZ) with resin cement. Materials and methods. Two different types of zirconia specimens with a fully sintered size of 14.0×14.0×2.0 mm³ were prepared, polished with 400, 600, and 800 grit silicon carbide paper, and buried in epoxy resin. They were classified into four groups each control, sandblasting, primer, and sandblasting & primer. Cylindrical resin adhered to the surface-treated zirconia with resin cement. It was stored in distilled water (37℃) for 24 hours, and a shear bond strength test was performed. The normality of the experimental group was confirmed with the Kolmogorov-Smirnov & Shapiro-Wilk test. The interaction and statistical difference were analyzed using a two-way ANOVA. A post-hoc analysis was performed using Dunnett T3. Results. As a result of two-way ANOVA, there was no significant difference in shear bonding strength between zirconia types (P > .05), but there was a significant correlation in the sandblasting, primer, and alumina sandblasting & primer group (P < .05). Dunnett T3 post-test showed that, regardless of the type of zirconia, shear bonding strength was sandblasting & primer > Primer > sandblasting > control group (P < .05). Conclusion. There was no difference in shear bond strength between the types of zirconia. The highest shear bond strength was shown when the mechanical and chemical treatments of the zirconia surface was performed simultaneously.

• Economic and Environmental Geology
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• v.8 no.3
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• pp.117-124
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• 1975

Wet chemical analysis (for $MnO_2$, MnO, and $H_2O$(+)) and electron microprobe analysis (for $Fe_2O_3$ and PbO) give $MnO_2$ 74.91, MnO 11.33, $Fe_2O_3$ (total Fe) 4.19, PbO 0.03, $H_2O$ (+) 9.46, sum 99.92%. 'Available oxygen determined by oxalate titration method is allotted to $MnO_2$ from total Mn, and the remaining Mn is calculated as MnO. Traces of Ba, Ca, Mg, K, Cu, Zn, and Al were found. Li and Na were not found. The existence of (OH) is verified from the infrared absorption spectra. The analysis corresponds to the formula $Mn^{4+}{_{4.85}}(Mn^{2+}{_{0.90}}Fe^{3+}{_{0.30}})_{1.20}O_{8.09}(OH)_{5.91}$, on the basis of O=14, 'or ideally $Mn^{4+}{_{5-x}}(Mn^{2+},Fe^{3+})_{1+x}O_{8}(OH)_{6}$ ($x{\approx}0.2$). X-ray single crystal study could not be made because of the distortion of single crystals. But the x-ray powder pattern is satisfactorily indexed by an orthorhombic cell with a 9.324, b 14.05, c $7.956{\AA}$., Z=4. The indexed powder diffraction lines are 9.34(s) (100), 7.09(s) (020), 4.62(m) (200, 121), 4.17(m) (130), 3.547(s) (112), 3.212(vw) (041), 3.101(s) (300), 2.597(w) (013), 2.469(m) (331), 2.214(vw)(420), 2.098(vw) (260), 2.014 (vw) (402), 1.863(w) (500), 1.664(w) (314), 1.554(vw) (600), 1.525(m) (601), 1.405(m) (0.10.0). DTA curve shows the endothermic peaks at $250-370^{\circ}C$ and $955^{\circ}C$. The former is due to the dehydration: and oxidation forming$(Mn,\;Fe)_2O_3$(cubic, a $9.417{\AA}$), and the latter is interpreted as the formation of a hausmannite-type oxide (tetragonal, a 5.76, c $9.51{\AA}$) from $(Mn,\;Fe)_2O_3$. Infrared absorption spectral curve shows Mn-O stretching vibrations at $515cm^{-1}$ and $545cm^{-1}$, O-H bending vibration at $1025cm^{-1}$ and O-H stretching vibration at $3225cm^{-1}$. Opaque. Reflectance 13-15%. Bireflectance distinct in air and strong in oil. Reflection pleochroism changes from whitish to light grey. Between crossed nicols, color changes from yellowish brown with bluish tint to grey in air and yellowish brown to grey through bluish brown in oil. No internal reflections. Etching reactions: HCl(conc.) and $H_2SO_4+H_2O_2$-grey tarnish; $SnCl_2$(sat.)-dark color; $HNO_3$(conc.)-grey color; $H_2O_2$-tarnish with effervescence. It is black in color. Luster dull. Cleavage one direction perfect. Streak brownish black to dark brown. H. (Mohs) 2-3, very fragile. Specific gravity 3.59(obs.), 3.57(calc.). It occurs as radiating groups of flakes, flower-like aggregates, colloform bands, dendritic or arborescent masses composed of fine grains in the cementation zone of the supergene manganese oxide deposits of the Janggun mine, Bonghwa-gun, southeastern Korea. Associated minerals are calcite, nsutite, todorokite, and some undetermined manganese dioxide minerals. The name is for the mine, the first locality. The mineral and name were approved before publication by the Commission on New Minerals and Mineral Names, I.M.A.