• Journal of the Korean Society for Heat Treatment
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• v.16 no.2
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• pp.71-77
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• 2003

We investigate the phase formation in the compound layer of cast irons during the gaseous nitrocarburising of four different cast irons, that contain different types of graphites in the shape and size. We examine the change in the surface roughness with the nitrocarburising time. The observation of cross-sectional microstructure and X-ray diffraction analysis indicate that the compound layer consists of single ${\varepsilon}-Fe_{2-3}(N,C)$ phase and that its thickness increases in a parabolic manner with the treatment time. The surface roughness parameters, Rz and Ra increase with increasing treatment time. In other words, the roughness parameters increase as the thickness of compound layer increases. The parameters also depend on the shape and size of graphite in the individual cast irons.

• Korean Journal of Materials Research
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• v.13 no.2
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• pp.88-93
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• 2003

Co/Ti bilayer structure in Co salicide process helps to the improvement of device speed by lowering contact resistance due to the epitaxial growth of $CoSi_2$layers. We investigated the epitaxial growth and interfacial mass transport of $CoSi_2$layers formed from $150 \AA$-Co/Ti structure with two step rapid thermal annealing (RTA). The thicknesses of Ti layers were varied from 20 $\AA$ to 100 $\AA$. After we confirmed the appropriate deposition of Ti film even below $100\AA$-thick, we investigated the cross sectional microstructure, surface roughness, eptiaxial growth, and mass transportation of$ CoSi_2$films formed from various Ti thickness with a cross sectional transmission electron microscopy XTEM), scanning probe microscopy (SPM), X-ray diffractometery (XRD), and Auger electron depth profiling, respectively. We found that all Ti interlayer led to$ CoSi_2$epitaxial growth, while $20 \AA$-thick Ti caused imperfect epitaxy. Ti interlayer also caused Co-Ti-Si compounds on top of $CoSi_2$, which were very hard to remove selectively. Our result implied that we need to employ appropriate Ti thickness to enhance the epitaxial growth as well as to lessen Co-Ti-Si compound formation.

• Korean Journal of Materials Research
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• v.15 no.5
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• pp.301-305
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• 2005

We fabricated nickel silicide layers on whole non-patterned wafers from $p-Si(100)SiO_2(200nm)$/poly-Si(70 nm)mn(40 nm) structure by 40 sec rapid thermal annealing of $500\~900^{\circ}C$. The sheet resistance, cross-sectional microstructure, surface roughness, and phase analysis were investigated by a four point probe, a field emission scanning electron microscope, a scanning probe microscope, and an X-ray diffractometer, respectively. Sheet resistance was as small as $7\Omega/sq$. even at the elevated temperature of $900^{\circ}C$. The silicide thickness and surface roughness increased as silicidation temperature increased. We confirmed the nickel silicides iron thin nickel/poly-silicon structures would be a mixture of NiSi and $NiSi_2$ even at the $NiSi_2$ stable temperature region.

• Korean Journal of Materials Research
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• v.16 no.9
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• pp.564-570
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• 2006

Silicides have been required to be below 40 nm-thick and to have low contact resistance without agglomeration at high silicidation temperature. We fabricated composite silicide layers on the wafers from Ni(20 nm)/Co(20 nm)/poly-Si(70 nm) structure by rapid thermal annealing of $700{\sim}1100^{\circ}C$ for 40 seconds. The sheet resistance, surface composition, cross-sectional microstructure, and surface roughness were investigated by a four point probe, a X-ray diffractometer, an Auger electron spectroscopy, a field emission scanning electron microscope, and a scanning probe microscope, respectively. The sheet resistance increased abruptly while thickness decreased as silicidation temperature increased. We propose that the fast metal diffusion along the silicon grain boundary lead to the poly silicon mixing and inversion. Our results imply that we may consider the serious thermal instability in designing and process for the sub-0.1 um CMOS devices.

• Journal of the Korean institute of surface engineering
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• v.28 no.6
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• pp.376-385
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• 1995

Copper-chromium multilayers with a nominal bilayer thickness of about 400 $\AA$ (200 $\AA$ each) were prepared by dc magnetron sputtering and the evolution of microstructure during heat treatment was investigated by using x-ray diffractometry(XRD), Auger electron spectroscopy(AES) and transmission electron microscopy(TEM). It was observed that an amorphous phase with a thickness of about 40 $\AA$ was formed at the interfaces of the as-deposited Cu/Cr multilayered film using cross-sectional TEM. At elevated temperatures, the Cu(111) reflection showed increasing intensity and decreasing line-width as a result of copper grain growth. The intermixed amorphous phase disappeared after annealing at $250^{\circ}C$ for 1 h and the multilayer structure was stable up to $400^{\circ}C$ for 1 h annealing. At $600^{\circ}C$ annealing, it was observed that the multilayer structure was completely destroyed and copper and chromium phases were fully intermixed.

• Journal of the Korean institute of surface engineering
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• v.35 no.6
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• pp.377-382
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• 2002

We investigated the appropriate wet cleaning process for Co-Ti-Si compounds formed on top of cobalt disilicide made from Co/Ti deposition and two rapid thermal annealing (RTA). We employed three wet cleaning processes, WP1 ($H_2$SO$_4$ etchant), WP2 ($NH_4$OH etchant), and WP3 which execute sequentially WP1 and WP2 after the first RTA. All samples were cleaned with BOE etchant after the second RTA. We characterized the sheet resistance with process steps by a four-point probe, the microstructure evolution by a cross detail sectional transmission electron microscope, a Auger depth profiler, and a X-ray diffractometer (XRD). We confirmed WP3 wet cleaning process were the most suitable to remove CoTiSi layer selectively.

• Korean Journal of Materials Research
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• v.26 no.12
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• pp.751-756
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• 2016

Graphite was diffusion-bonded by hot-pressing to W-25Re alloy using a Ti interlayer. For the joining, a uniaxial pressure of 25 MPa was applied at $1600^{\circ}C$ for 2 hrs in an argon atmosphere with a heating rate of $10^{\circ}C\;min^{-1}$. The interfacial microstructure and elemental distribution of the W-25Re/Ti/Graphite joints were analyzed by scanning electron microscopy (SEM). Hot-pressed joints appeared to form a stable interlayer without any micro-cracking, pores, or defects. To investigate the high-temperature stability of the W-25Re/Ti/Graphite joint, an oxy-acetylene torch test was conducted for 30 seconds with oxygen and acetylene at a 1.3:1 ratio. Cross-sectional analysis of the joint was performed to compare the thickness of the oxide layer and its chemical composition. The thickness of W-25Re changed from 250 to $20{\mu}m$. In the elemental analysis, a high fraction of rhenium was detected at the surface oxidation layer of W-25Re, while the W-25Re matrix was found to maintain the initial weight ratio. Tungsten was first reacted with oxygen at a torch temperature over $2500^{\circ}C$ to form a tungsten oxide layer on the surface of W-25Re. Then, the remaining rhenium was subsequently reacted with oxygen to form rhenium oxide. The interfacial microstructure of the Ti-containing interlayer was stable after the torch test at a temperature over $2500^{\circ}C$.

• Korean Journal of Materials Research
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• v.13 no.1
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• pp.43-47
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• 2003

As and BF$_2$dopants are implanted for the formation of source/drain with dose of 1${\times}$10$^{15}$ ions/$\textrm{cm}^2$∼5${\times}$10$^{15}$ ions/$\textrm{cm}^2$ then formed cobalt disilicide with Co/Ti deposition and doubly rapid thermal annealing. Appropriate ion implantation and cobalt salicide process are employed to meet the sub-0.13 $\mu\textrm{m}$ CMOS devices. We investigated the process results of sheet resistance, dopant redistribution, and surface-interface microstructure with a four-point probe, a secondary ion mass spectroscope(SIMS), a scanning probe microscope (SPM), and a cross sectional transmission electron microscope(TEM), respectively. Sheet resistance increased to 8%∼12% as dose increased in $CoSi_2$$n^{＋}$ and $CoSi_2$$p^{V}$ , while sheet resistance uniformity showed very little variation. SIMS depth profiling revealed that the diffusion of As and B was enhanced as dose increased in $CoSi_2$$n^{＋}$ and $CoSi_2$$p^{＋}$ . The surface roughness of root mean square(RMS) values measured by a SPM decreased as dose increased in $CoSi_2$$n^{＋}$ , while little variation was observed in $CoSi_2$$p^{＋}$ . Cross sectional TEM images showed that the spikes of 30 nm∼50 nm-depth were formed at the interfaces of $CoSi_2$$n^{＋}$ / and $CoSi_2$/$p^{＋}$, which indicate the possible leakage current source. Our result implied that Co/Ti cobalt salicide was compatible with high dose sub-0.13$\mu\textrm{m}$ process.

• Applied Microscopy
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• v.43 no.2
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• pp.88-97
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• 2013

Technical investigation to figure out the problems arising during in-situ heating electron backscatter diffraction (EBSD) analysis inside scanning electron microscopy (SEM) was carried out. EBSD patterns were successfully acquired up to $830^{\circ}C$ without degradation of EBSD pattern quality in steels. Several technical problems such as image drift and surface microstructure pinning were taking place during in-situ experiments. Image drift problem was successfully prevented in constant current supplying mode. It was revealed that the surface pinning problem was resulted from the $TiO_2$ oxide particle formation during heating inside SEM chamber. Surface pinning phenomenon was fairly reduced by additional platinum and carbon multi-layer coating before in-situ heating experiment, furthermore was perfectly prevented by improvement of vacuum level of SEM chamber via leakage control. Plane view in-situ observation provides better understanding on the overall feature of recrystallization phenomena and cross sectional in-situ observation provides clearer understanding on the recrystallization mechanism.

• Progress in Superconductivity
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• v.9 no.1
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• pp.96-101
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• 2007

[ $YBa_2Cu_3O_{7-{\delta}}$ ] films have been prepared on $LaAlO_3$ (100) single-crystal substrates by a metalorganic deposition using dichloroacetate precursors (DCA-MOD). Calcination conditions were varied in order to optimize the microstructure and the superconducting properties of YBCO film. Coated films were calcined at various temperatures ranging from $400{\sim}700^{\circ}C$ in flowing humid oxygen atmosphere. Ramping rate to calcination tempertures was $2.22^{\circ}C/min$. Conversion heat treatment was performed at $800^{\circ}C$ for 2 h in flowing Ar gas containing 1000 ppm oxygen with a humidity of 9.45%. Observations of surface and cross sectional SEM microstructure showed that the particle size in the calcined film increased in the range of 100-200 nm with heating rate and the calcination temperature. SEM EDS analysis showed that 13 a/o of chlorine was contained in the calcined film. It was also observed that the porosity increased with the heating rate and temperature. Porous microstructure was developed when YBCO films were prepared using porous calcined film. Dense microstructure and high $J_c$ over $1\;MA/cm^2$ was obtained when calcination was carried out at the temperature of $500^{\circ}C$ with a heating rate of $2.22^{\circ}C/min$.