• Korean Journal of Materials Research
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• v.12 no.3
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• pp.211-214
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• 2002

Properties of 52/48 PZT films with various thicknesses for piezoelectric micro-electro mechanical systems (MEMS) devices fabricated by multi-coating method on $Pt(3500{\AA})/Ti(400{\AA})/SiO_2(3000{\AA})/Si$(525$\mu\textrm{m}$) substrates were investigated. PZT films were deposited by spin-coating process at 3500 rpm for 30 sec, followed by pyrolysis at 45$0^{\circ}C$ for 10 min producing the thickness of about 120nm. These processes were repeated 4, 8, 12, 16 and 20 times in order to have various thicknesses, respectively. Finally, they were crystallized at $650^{\circ}C$ for 30 min. All thick PZT films showed dense and homogeneous surface microstructures. Thick PZT films showed crystalline structures of random orientations with increasing thickness. Dielectric constants of thick PZT films were increased with increasing film thickness and reached 800 at 100kHz for 2.3$\mu\textrm{m}$ thick PZT film. $P_r\; and\; E_c$ of 2.3$\mu\textrm{m}$ thick PZT films were about 20$\mu$C/$\textrm{cm}^2$ and 63kV/cm. Depth profile analysis by Auger Electron Spectroscopy (AES) of 4800 $\AA$ thick PZT film showed the formation of the perovskite phase on Pt layer by Pb diffusion behavior. It was considered that Pb-Pt intermediate layer promoted PZT (111) columnar structures.

• Korean Journal of Materials Research
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• v.9 no.11
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• pp.1148-1152
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• 1999

An organometallic precursor, hfac(hexafluoroacetylacetonate) Cu(I) DMB (3,3-dimethyl- 1-butene) was synthesized, evaluated and compared with other precursors for metal organic chemical vapor deposition of copper thin films. It was found that at $40^{\circ}C$, the vapor pressure was an order of magnitude higher (about 3 torr) than (hfac) Cu vinyltrimethylsilane (VTMS) and films could be deposited at the substrate temperature of 100-$280^{\circ}C$ with deposition rate substantially higher. The copper films contained no detectable impurities as measured by Auger electron spectroscopy and had a resistivity of about 2.0$\mu\Omega$-cm in the deposition temperature range of 150 to $250^{\circ}C$. From the thermal analysis, (hfac)Cu(I)(DMB) is believed to be quite stable and no appreciable amount of precipitation was observed at $65^{\circ}C$ heating for more than a month.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.06a
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• pp.8-9
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• 2006

Hafnium oxide ($HfO_2$) thin films were deposited on p-type (100) silicon wafers by atomic layer deposition (ALD) using TEMAHf and $O_3$. Prior to the deposition of $HfO_2$ films, a thin Hf ($10\;{\AA}$) metal layer was deposited. Deposition temperature of $HfO_2$ thin film was $350^{\circ}C$ and its thickness was $150\;{\AA}$. Samples were then annealed using furnace heating to temperature ranges from 500 to $900^{\circ}C$. The MOS capacitor of round-type was fabricated on Si substrates. Thermally evaporated $3000\;{\AA}$-thick AI was used as top electrode. In this work, We study the interface characterization of $HfO_2$/Hf/Si MOS capacitor depending on annealing temperature. Through AES(Auger Electron Spectroscopy), capacitance-voltage (C-V) and current-voltage (I-V) analysis, the role of Hf layer for the better $HfO_2$/Si interface property was investigated. We found that Hf meta1 layer in our structure effective1y suppressed the generation of interfacial $SiO_2$ layer between $HfO_2$ film and silicon substrate.

• The Journal of Korean Academy of Prosthodontics
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• v.42 no.3
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• pp.307-326
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• 2004

Statement of problem. The long-term success of implants is the development of a stable direct connection between bone and implant surface, which must be structural and functional. To improve a direct implant fixation to the bone, various strategies have been developed focusing on the surface of materials. Among them, altering the surface properties can modify cellular responses such as cell adhesion, cell motility and bone deposition. Purpose. This study was to evaluate the cellular behaviors on the surface-modified titanium by morphological observation, cellular proliferation and differentiation. Material and methods. Specimens were divided into five groups, depending on their surface treatment: electropolishing(EP) anoclizing(AN), machining(MA), blasting with hydroxyapatite particle(RBM) and electrical discharge machining(EDM). Physicochemical properties and microstructures of the specimens were examined and the responses of osteoblast-like cells were investigated. The microtopography of specimens was observed by scanning electron microscopy(SEM). Surface roughness was measured by a three-dimensional roughness measuring system. The microstructure was analyzed by X-ray diffractometer(XRD) and scanning auger electron microscopy(AES). To evaluate cellular responses to modified titanium surfaces, osteoblasts isolated from neonatal rat were cultured. The cellular morphology and total protein amounts of osteoblast-like cell were taken as the marker for cellular proliferation, while the expression of alkaline phosphatase was used as the early differentiation marker for osteoblast. In addition, the type I collagen production was determined to be a reliable indicator of bone matrix synthesis. Results. 1. Each prepared specimen showed specific microtopography at SEM examination. The RBM group had a rough and irregular pattern with reticulated appearance. The EDM-treated surface had evident cracks and was heterogeneous consisting of broad sheet or plate with smooth edges and clusters of small grains, deep pores or craters. 2. Surface roughness values were, from the lowest to the highest, electropolished group, anodized group, machined group, RBM group and EDM group. 3. All groups showed amorphous structures. Especially anodized group was found to have increased surface oxide thickness and EDM group had titaniumcarbide(TiC) structure. 4. Cells on electropolished, anodized and machined surfaces developed flattened cell shape and cells on RBM appeared spherical and EDM showed both. After 14 days, the cells cultured from all groups were formed to be confluent and exhibited multilayer proliferation, often overlapped or stratified. 5. Total protein amounts were formed to be quite similar among all the group at 48 hours. At 14 days, the electropolished group and the anodized group induced more total protein amount than the RBM group(P<.05). 6. There was no significant difference among five groups for alkaline phosphatase(ALP) activity at 48 hours. The AN group showed significantly higher ALP activity than any other groups at 14 days(P<.05). 7. All the groups showed similar collagen synthesis except the EDM group. The amount of collagen on the electropolished and anodized surfaces were higher than that on the EDM surface(P<.05).

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.155.2-155.2
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• 2013

Strain-relaxed SiGe layer on Si substrate has numerous potential applications for electronic and opto- electronic devices. SiGe layer must have a high degree of strain relaxation and a low dislocation density. Conventionally, strain-relaxed SiGe on Si has been manufactured using compositionally graded buffers, in which very thick SiGe buffers of several micrometers are grown on a Si substrate with Ge composition increasing from the Si substrate to the surface. In this study, a new plasma process, i.e., the combination of PIII&D and HiPIMS, was adopted to implant Ge ions into Si wafer for direct formation of SiGe layer on Si substrate. Due to the high peak power density applied the Ge sputtering target during HiPIMS operation, a large fraction of sputtered Ge atoms is ionized. If the negative high voltage pulse applied to the sample stage in PIII&D system is synchronized with the pulsed Ge plasma, the ion implantation of Ge ions can be successfully accomplished. The PIII&D system for Ge ion implantation on Si (100) substrate was equipped with 3'-magnetron sputtering guns with Ge and Si target, which were operated with a HiPIMS pulsed-DC power supply. The sample stage with Si substrate was pulse-biased using a separate hard-tube pulser. During the implantation operation, HiPIMS pulse and substrate's negative bias pulse were synchronized at the same frequency of 50 Hz. The pulse voltage applied to the Ge sputtering target was -1200 V and the pulse width was 80 usec. While operating the Ge sputtering gun in HiPIMS mode, a pulse bias of -50 kV was applied to the Si substrate. The pulse width was 50 usec with a 30 usec delay time with respect to the HiPIMS pulse. Ge ion implantation process was performed for 30 min. to achieve approximately 20 % of Ge concentration in Si substrate. Right after Ge ion implantation, ~50 nm thick Si capping layer was deposited to prevent oxidation during subsequent RTA process at $1000^{\circ}C$ in N2 environment. The Ge-implanted Si samples were analyzed using Auger electron spectroscopy, High-resolution X-ray diffractometer, Raman spectroscopy, and Transmission electron microscopy to investigate the depth distribution, the degree of strain relaxation, and the crystalline structure, respectively. The analysis results showed that a strain-relaxed SiGe layer of ~100 nm thickness could be effectively formed on Si substrate by direct Ge ion implantation using the newly-developed PIII&D process for non-gaseous elements.

• Korean Journal of Materials Research
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• v.2 no.6
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• pp.408-416
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• 1992

Stable TiS$i_2$was formed by RTA on single-Si and on poly-Si. Subsequently, an Al-1% Si layer with 600-nm thick was deposited on top of the TiS$i_2$, Finally, the specimens were annealed for 30min at 400-60$0^{\circ}C$in $N_2$ambient. The thermal stability of Al-1% Si/TiS$i_2$bilayer and interfacial reaction were investigated by measuring sheet resistance, Auger electron spectroscopy (AES), and scanning electron microscopy (SEM). The composition and phase of precipitates formed by the reaction of Al-1% Si with Ti-silicide were studied by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD). In the case of single-Si substrate the reaction of Al-1% Si layer with TiS$i_2$layer resulted in precipitates, consuming all TiS$i_2$layer at 55$0^{\circ}C$. On the other hand, the disappearance of TiS$i_2$on poly-Si occurred at 50$0^{\circ}C$ and more precipitates were formed by the reaction of Al-1% Si/TiS$i_2$on potty-Si substrate than those of the reaction on single-Si substrate. This phenomenon resulted from the fact that Ti-silicide formed on poly-Si was more unstable than on single-Si by the effect of grain boundary. By EDS analysis the precipitates were found tobe composed of Ti, Al, and Si. X-ray diffraction showed the phase of precipitates to be theT$i_7$A$l_5$S$i_12$ternary compound.

• Journal of the Korean Ceramic Society
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• v.31 no.12
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• pp.1577-1587
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• 1994

TiO2 thin films with the substitution of oxygen with nitrogen were deposited on silicon substrate by metalorganic chemical vapor deposition (MOCVD) using Ti(OCH(CH3)2)4 (titanium tetraisopropoxide, TTIP) and N2O as source materials. X-ray diffraction (XRD) results indicated that the crystal structure of the deposited thin films was anatase TiO2 with only (101) plane observed at the deposition temperatures of 36$0^{\circ}C$ and 38$0^{\circ}C$, and with (101) and (200) plane at above 40$0^{\circ}C$. Raman spectroscopic results indicated that the crystal structure was anatase TiO2 in accordance with the XRD results without any rutile, fcc TiN, or hcp TiN structure. No fundamental difference was observed with temperature increase, but the peak intensity at 194.5 cm-1 increased with strong intensity at 143.0 cm-1 for all samples. The crystalline size of the films varied from 49.2 nm to 63.9 nm with increasing temperature as determined by slow-scan XRD experiments. The refractive index of the films increased from 2.40 to 2.55 as temperature increased. X-ray photoelectron spectroscopy (XPS) study showed only Ti 2s, Ti 2p, C 1s, O 1s and O 2s peaks at the surface of the film. The composition of the surface was estimated to be TiO1.98 from the quatitative analysis. In the bulk of the film Ti 2s, Ti 2p, O 1s, O 2s, N 1s and N 2s were detected, and Ti-N bonding was observed due to the substitution of oxygen with nitrogen. A satellite structure was observed in the Ti 2p due to the Ti-N bonding, and the composition of titanium nitride was determined to be about TiN1.0 from the position of the binding energy of Ti-N 2p3/2 and the quatitative analysis. The spectrum of Ti 2p energy level could be the sum of a 4, 5, or 6 Gaussian curve reconstruction, and the case of the sum of the 6 Gaussian curve reconstruction was physically most meaningful. From the results of Auger electron spectroscopy (AES), it was known that the composition was not varied significantly throughout the whole thickness of the film, and silicon oxide was not observed at the interface between the film and the substrate. The composition of the film was possible (TiO2)1-x.(TiN)x or TiO2-2xNx and in this experimental condition x was found to be about 0.21-0.16.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.239-240
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• 2008

As semiconductor devices are scaled down for better performance and more functionality, the Cu-based interconnects suffer from the increase of the resistivity of the Cu wires. The resistivity increase, which is attributed to the electron scattering from grain boundaries and interfaces, needs to be addressed in order to further scale down semiconductor devices [1]. The increase in the resistivity of the interconnect can be alleviated by increasing the grain size of electroplating (EP)-Cu or by modifying the Cu surface [1]. Another possible solution is to maximize the portion of the EP-Cu volume in the vias or damascene structures with the conformal diffusion barrier and seed layer by optimizing their deposition processes during Cu interconnect fabrication, which are currently ionized physical vapor deposition (IPVD)-based Ta/TaN bilayer and IPVD-Cu, respectively. The use of in-situ etching, during IPVD of the barrier or the seed layer, has been effective in enlarging the trench volume where the Cu is filled, resulting in improved reliability and performance of the Cu-based interconnect. However, the application of IPVD technology is expected to be limited eventually because of poor sidewall step coverage and the narrow top part of the damascene structures. Recently, Ru has been suggested as a diffusion barrier that is compatible with the direct plating of Cu [2-3]. A single-layer diffusion barrier for the direct plating of Cu is desirable to optimize the resistance of the Cu interconnects because it eliminates the Cu-seed layer. However, previous studies have shown that the Ru by itself is not a suitable diffusion barrier for Cu metallization [4-6]. Thus, the diffusion barrier performance of the Ru film should be improved in order for it to be successfully incorporated as a seed layer/barrier layer for the direct plating of Cu. The improvement of its barrier performance, by modifying the Ru microstructure from columnar to amorphous (by incorporating the N into Ru during PVD), has been previously reported [7]. Another approach for improving the barrier performance of the Ru film is to use Ru as a just seed layer and combine it with superior materials to function as a diffusion barrier against the Cu. A RulTaN bilayer prepared by PVD has recently been suggested as a seed layer/diffusion barrier for Cu. This bilayer was stable between the Cu and Si after annealing at $700^{\circ}C$ for I min [8]. Although these reports dealt with the possible applications of Ru for Cu metallization, cases where the Ru film was prepared by atomic layer deposition (ALD) have not been identified. These are important because of ALD's excellent conformality. In this study, a bilayer diffusion barrier of Ru/TaCN prepared by ALD was investigated. As the addition of the third element into the transition metal nitride disrupts the crystal lattice and leads to the formation of a stable ternary amorphous material, as indicated by Nicolet [9], ALD-TaCN is expected to improve the diffusion barrier performance of the ALD-Ru against Cu. Ru was deposited by a sequential supply of bis(ethylcyclopentadienyl)ruthenium [Ru$(EtCp)_2$] and $NH_3$plasma and TaCN by a sequential supply of $(NEt_2)_3Ta=Nbu^t$ (tert-butylimido-trisdiethylamido-tantalum, TBTDET) and $H_2$ plasma. Sheet resistance measurements, X-ray diffractometry (XRD), and Auger electron spectroscopy (AES) analysis showed that the bilayer diffusion barriers of ALD-Ru (12 nm)/ALD-TaCN (2 nm) and ALD-Ru (4nm)/ALD-TaCN (2 nm) prevented the Cu diffusion up to annealing temperatures of 600 and $550^{\circ}C$ for 30 min, respectively. This is found to be due to the excellent diffusion barrier performance of the ALD-TaCN film against the Cu, due to it having an amorphous structure. A 5-nm-thick ALD-TaCN film was even stable up to annealing at $650^{\circ}C$ between Cu and Si. Transmission electron microscopy (TEM) investigation combined with energy dispersive spectroscopy (EDS) analysis revealed that the ALD-Ru/ALD-TaCN diffusion barrier failed by the Cu diffusion through the bilayer into the Si substrate. This is due to the ALD-TaCN interlayer preventing the interfacial reaction between the Ru and Si.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.251-252
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• 2012

Recently, the growing interest in organic microelectronic devices including OLEDs has led to an increasing amount of research into their many potential applications in the area of flexible electronic devices based on plastic substrates. However, these organic devices require a gas barrier coating to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency OLEDs require an extremely low Water Vapor Transition Rate (WVTR) of $1{\times}10^{-6}g/m^2$/day. The Key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required ($1{\times}10^{-6}g/m^2$/day) is the suppression of defect sites and gas diffusion pathways between grain boundaries. In this study, we developed an $Al_2O_3$ nano-crystal structure single gas barrier layer using a Neutral Beam Assisted Sputtering (NBAS) process. The NBAS system is based on the conventional RF magnetron sputtering and neutral beam source. The neutral beam source consists of an electron cyclotron Resonance (ECR) plasma source and metal reflector. The Ar+ ions in the ECR plasma are accelerated in the plasma sheath between the plasma and reflector, which are then neutralized by Auger neutralization. The neutral beam energies were possible to estimate indirectly through previous experiments and binary collision model. The accelerating potential is the sum of the plasma potential and reflector bias. In previous experiments, while adjusting the reflector bias, changes in the plasma density and the plasma potential were not observed. The neutral beam energy is controlled by the metal reflector bias. The NBAS process can continuously change crystalline structures from an amorphous phase to nano-crystal phase of various grain sizes within a single inorganic thin film. These NBAS process effects can lead to the formation of a nano-crystal structure barrier layer which effectively limits gas diffusion through the pathways between grain boundaries. Our results verify the nano-crystal structure of the NBAS processed $Al_2O_3$ single gas barrier layer through dielectric constant measurement, break down field measurement, and TEM analysis. Finally, the WVTR of $Al_2O_3$ nano-crystal structure single gas barrier layer was measured to be under $5{\times}10^{-6}g/m^2$/day therefore we can confirm that NBAS processed $Al_2O_3$ nano-crystal structure single gas barrier layer is suitable for OLED application.

• Korean Journal of Materials Research
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• v.19 no.2
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• pp.61-67
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• 2009

Electrolessly deposited Co (Re,P) was investigated as a possible capping layer for Cu wires. 50 nm Co (Re,P) films were deposited on Cu/Ti-coated silicon wafers which acted as a catalytic seed and an adhesion layer, respectively. To obtain the optimized bath composition, electroless deposition was studied through an electrochemical approach via a linear sweep voltammetry analysis. The results of using this method showed that the best deposition conditions were a $CoSO_4$ concentration of 0.082 mol/l, a solution pH of 9, a $KReO_4$ concentration of 0.0003 mol/l and sodium hypophosphite concentration of 0.1 mol/L at $80^{\circ}C$. The thermal stability of the Co (Re,P) layer as a barrier preventing Cu was evaluated using Auger electron spectroscopy and a Scanning calorimeter. The measurement results showed that Re impurities stabilized the h.c.p. phase up to $550^{\circ}C$ and that the Co (Re,P) film efficiently blocked Cu diffusion under an annealing temperature of $400^{\circ}C$ for 1hr. The good barrier properties that were observed can be explained by the nano-sized grains along with the blocking effect of the impurities at the fast diffusion path of the grain boundaries. The transformation temperature from the amorphous to crystal structure is increased by doping the Re.