• Journal of the Korea Academia-Industrial cooperation Society
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• v.8 no.1
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• pp.25-32
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• 2007

We investigated the silicide reaction stability between 10 nm-Col-xNix alloy films and silicon substrates with the existence of 4 nm-thick natural oxide layers. We thermally evaporated 10 nm-Col-xNix alloy films by varying $x=0.1{\sim}0.9$ on naturally oxidized single crystal and 70 nm-thick polycrystalline silicon substrates. The films structures were annealed by rapid thermal annealing (RTA) from $600^{\circ}C$ to $1100^{\circ}C$ for 40 seconds with the purpose of silicidation. After the removal of residual metallic residue with sulfuric acid, the sheet resistance, microstructure, composition, and surface roughness were investigated using a four-point probe, a field emission scanning electron microscope, a field ion bean4 an X-ray diffractometer, and an Auger electron depth profiling spectroscope, respectively, to confirm the silicide reaction. The residual stress of silicon substrate was also analyzed using a micro-Raman spectrometer We report that the silicide reaction does not occur if natural oxides are present. Metallic oxide residues may be present on a polysilicon substrate at high silicidation temperatures. Huge residual stress is possible on a single crystal silicon substrate at high temperature, and these may result in micro-pinholes. Our results imply that the natural oxide layer removal process is of importance to ensure the successful completion of the silicide process with CoNi alloy films.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.234-234
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• 2010

최근 CMOS 소자 크기가 축소됨에 따라 소스와 드레인 영역에서의 접촉저항을 줄이기 위하여, 실리사이드 공정이 많이 연구되고 있다. 실리사이드 물질로서 NiSi는 낮은 저항률과 낮은 실리콘 소모, 낮은 공정온도, 등의 장점을 가지고 있다. 그러나, 실리사이드 형성으로 인한 나노소자의 소오스/드레인에서정션(junction) 누설전류의 증가는 큰 문제가 되므로 실리콘과 실리사이드 계면의 특성이 중요하다. 본 연구에서는 니켈을 이용한 실리사이드 형성시 계면 활성제인 에틸 요오드를 이용하여 실험을 진행하였다. 금속 유기 전구체인 MABONi을 사용하여 ALD 방식으로 증착 한 니켈 박막과 니켈 핵 형성시 계면활성제인 에틸요오드의 처리 방법에 따른 Ni-silicide 박막의 특성을 비교, 분석하였다. 먼저 자연산화막을 건식식각으로 제거한 뒤, 첫 번째 샘플에서는 10회의 주기로 초기 니켈을 증착한 뒤, 에틸요오드로 니켈의 표면 위를 처리하고, 다시 200회의 주기로 니켈을 증착하였으며, 두 번째는 첫 번째 방식에서 에틸요오드 주입 시 동시에 수소도 함께 주입하였다. 세 번째는 비교를 위해 에틸요오드 처리를 하지 않고 니켈 박막만을 증착 하였다. 이어서, 각 샘플을 급속 열처리 장비에서 $400^{\circ}C$부터 $900^{\circ}C$까지 각각 30sec간 열처리를 진행후, 반응하지 않은 잔여 니켈을 제거한 후, XRD(x-ray diffraction), AES(auger), 그리고 4-point probe 등을 이용하여 형성된 실리사이드의 특성을 분석하였다. 에틸요오드와 함께 수소를 주입한 경우 계면에서의 산소 불순물과 카본 성분이 효과적으로 제거되어 $400^{\circ}C$에서 $2.9{\Omega}/{\Box}$ 의 낮은 면저항을 가지는 NiSi가 형성되었고 모든 온도구간에서 다른 샘플에 비하여 가장 낮은 면저항 분포를 보였다. 이는 분해 흡착된 요오드에 의한 계면 특성 향상과 카본 성분이 포함된 잔여물들이 수소처리에 의해 효율적으로 제거되어 실리사이드의 특성이 향상되었기 때문이다. 계면활성제를 사용하지 않은 경우에는 $500^{\circ}C$에서 NiSi가 형성되었다. 반면에 에틸요오드로만 표면을 처리한 경우에는 니켈과 실리콘 계면에서의 카본 성분에 의하여 silicidation 이 충분히 일어나지 않았다. 이러한 결과는 향후 45nm 이하의 CMOS 공정상에서 소스와 드레인의 낮은 누설전류를 가지고, 접촉저항을 줄이기 위한 니켈 실리사이드 형성에 큰 도움을 줄 것으로 기대된다.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.08a
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• pp.78-78
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• 2013

Recently, many platinoid metals like platinum and ruthenium have been used as an electrode of microelectronic devices because of their low resistivity and high work-function. However the material cost of Ru is very expensive and it usually takes long initial nucleation time on SiO2 during chemical deposition. Therefore many researchers have focused on how to enhance the initial growth rate on SiO2 surface. There are two methods to deposit Ru film with atomic layer deposition (ALD); the one is thermal ALD using dilute oxygen gas as a reactant, and the other is plasma enhanced ALD (PEALD) using NH3 plasma as a reactant. Generally, the film roughness of Ru film deposited by PEALD is smoother than that deposited by thermal ALD. However, the plasma is not favorable in the application of high aspect ratio structure. In this study, we used a bis(ethylcyclopentadienyl)ruthenium [Ru(EtCp)2] as a metal organic precursor for both thermal and plasma enhanced ALDs. In order to reduce initial nucleation time, we use several methods such as Ar plasma pre-treatment for PEALD and usage of sacrificial RuO2 under layer for thermal ALD. In case of PEALD, some of surface hydroxyls were removed from SiO2 substrate during the Ar plasma treatment. And relatively high surface nitrogen concentration after first NH3 plasma exposure step in ALD process was observed with in-situ Auger electron spectroscopy (AES). This means that surface amine filled the hydroxyl removed sites by the NH3 plasma. Surface amine played a role as a reduction site but not a nucleation site. Therefore, the precursor reduction was enhanced but the adhesion property was degraded. In case of thermal ALD, a Ru film was deposited from Ru precursors on the surface of RuO2 and the RuO2 film was reduced from RuO2/SiO2 interface to Ru during the deposition. The reduction process was controlled by oxygen partial pressure in ambient. Under high oxygen partial pressure, RuO2 was deposited on RuO2/SiO2, and under medium oxygen partial pressure, RuO2 was partially reduced and oxygen concentration in RuO2 film was decreased. Under low oxygen partial pressure, finally RuO2 was disappeared and about 3% of oxygen was remained. Usually rough surface was observed with longer initial nucleation time. However, the Ru deposited with reduction of RuO2 exhibits smooth surface and was deposited quickly because the sacrificial RuO2 has no initial nucleation time on SiO2 and played a role as a buffer layer between Ru and SiO2.

• Journal of the Mineralogical Society of Korea
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• v.19 no.1 s.47
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• pp.31-38
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• 2006

Site environments bring about various different deterioration forms of stone cultural properties. The aim of this study is to document the influence of coarse grained sandy soil on the deterioration of stone cultural properties. Bulguksadabotap is a good example that demonstrates the problem with coarse grained sandy soil. The ground around the Bulguksadabotap is covered with coarse grained sandy soil and the pagoda is surrounded by the corridors. Coarse grained sandy soil float easily in the air and deposit in the complicated stone structure caused by strong wind in Gyeongju and numerous visitors. To explain the influence of coarse grained sandy soil on the deterioration, the coarse grained sandy soil and weathered stone pieces of Bulguksadabotap were analyzed by XRD, optical microscopy, SEM for mineralogical component and IC and ICP-AES for the soluble salts. The soil and weathered stone pieces include clay minerals, such as smectite and kaolinite, can expand with water and exert pressure on the stone. Small size of the clay minerals in the coarse grained sandy soil can easily penetrate into the weathered surfaces of the Bulguksadabotap. The weathered stone pieces also contain NaCl, which is known to contribute to increase the expandibility of clay minerals by providing with $Na^{+}$ or by dropping the equilibrium of relative humidity. These results indicates that coarse grained sandy soil is not proper to site environment for weathered stone cultural properties.

• Korean Journal of Materials Research
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• v.9 no.3
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• pp.244-250
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• 1999

MOCVD TiN films were prepared from a new TiN precursor, tetrakis(etylmethylamino)titanium (TEMAT) and ammonia. Deposition of TiN films from a single precursor, TEMA T yielded the growth rates of $70 to 1050\AA$/min, depending on the deposition temperature. Furthermore, the excellent bottom coverage of -90% over $0.35\mu\textrm{m}$ contacts was obtained at $275^{\circ}C$. The addition of ammonia to TEMA T lowered the resistivity of as- deposited TiN film to ~ $800\mu\omega-cm$ from $3500~6000\mu\omega-cm$ and improved the stability of TiN film in air. Examination of the films by Auger electron spectroscopy(AES) showed that the oxygen and carbon contents decreased with the addition of ammonia. However, increasing ammonia flow rate decreased the bottom coverage of TiN films over $0.5\mu\textrm{m}$ contacts, probably due to the high sticking coefficient of intermediate species produced from the gas phase reaction of TEMA T and ammonia. Based on the byproduct gases detected by the quadrupole mass spectrometer (QMS), the transammination reaction was proposed to be responsible for TiN deposition. In addition, XPS analysis revealed that the carbon in the films made from TEMA T and ammonia was metallic carbon, suggesting that $\beta$-hydrogen activation process occurs competitively with the transammination reaction.

• Korean Journal of Food Science and Technology
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• v.32 no.6
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• pp.1442-1445
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• 2000

This study was carried out to investigate the contents of minerals and heavy metals in the sea salts of Korean products and imported products. NaCl was major component, which ranged from $80.31{\sim}89.84%$ for Korean products and from $91.59{\sim}97.66%$ for imported products. Minerals and heavy metals of Korean products and imported products were analyzed with ICP-AES and AAS, respectively. Mineral contents of K and Mg in Korean products were relatively higher than those in imported ones, but no significant differences were found for heavy metals between them.

• Resources Recycling
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• v.26 no.4
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• pp.50-55
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• 2017

Determination of trace elements in a sample including complicated matrix is very difficult due to the interference by the matrix. Therefore, if the trace elements can be separated from the complex sample matrix and determined, the interference effects can be reduced, and it is very helpful for the overall analysis. In this study, the analytes of trace elements were separated from the sample matrix by co-precipitation with trace elements using indium hydroxide ($In(OH)_3$), then detected by inductively coupled plasma-atomic emission spectrometer (ICP-AES). Above all, the optimal conditions for the co-precipitation of elements with indium hydroxide were experimentally established. At last, salt was analyzed by the developed analytical method. No heavy metals were not found in Shinan Jeungdo salt, but trace amounts of several heavy metals except for cadmium were found in Cheonnam Yongkwang salt.

• Korean Journal of Materials Research
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• v.4 no.5
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• pp.550-555
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• 1994

The effects of RTA treatment on the leakage current have been studied for tantalum pentoxide( $Ta_2O_5$) films deposited by PECVD on P-type(100) Si substrate using $TaCl_5$(99.99%) and $N_2O$(99.99%) gaseous mixture. The refractive index increased with increasing the deposition temperature and the maximum deposition rate was obtained at $500^{\circ}C$. The Ta-0 bond peak intensity of as-deposited $Ta_2O_5$ increased with increasing the deposition temperature through FT-IR analysis and the leakage current value was decreased with increasing the deposition temperature. The small leakage current value obtained after RTA treatment of as-deposited $Ta_2O_5$ was found to be due to the reduction of 0-deficient structure in the film. The increases of the oxygen coacentration and the Ta-0 bond peak intensity in the film after RTA treatment were measured by AES and FT-IR analyses.

• Applied Chemistry for Engineering
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• v.22 no.3
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• pp.255-260
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• 2011

$NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina which is expected to an inorganic solid electrolyte of high temperature polymer electrolyte membrane fuel cells (PEMFC) was prepared by ion-exchange reaction of $K^{+}-{\beta}^{{\prime}{\prime}}$-alumina pellet with $NH_4NO_3$ aqueous solution and molten $NH_4NO_3$ salts as an ion-exchange medium in the autoclave and the heating mentle reaction. In the autoclave reaction, the concentrations of $NH_4NO_3$ solution was chosen at 5 and 10 M. Each ion-exchange reaction was carried out at 130, 150, 170, and $200^{\circ}C$ for 2, 4, 6 and 8 h. In the heating mentle reaction, ion-exchange was performed at $200^{\circ}C$ for 2, 4, 6 and 8 h with molten $NH_4NO_3$ salts. In order to determine the effect of reaction times, each ion-exchange reaction was repeated 3 times. The phase stability and the ion-exchange rate of $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina were analyzed by XRD and ICP.

• Clean Technology
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• v.26 no.4
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• pp.270-278
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• 2020

Palladium (Pd) has been widely used in various industrial applications such as jewelry, catalyst, and dental materials despite its limited resources. It has been gaining attention to recover Pd with high purity from the spent materials. This study investigated the optimum conditions for the leaching and recovery of metallic Pd. The leaching parameters are HCl concentration, temperature, time, concentration of oxidants, and pulp density. 97.2% of Pd leaching efficiency was obtained in 3 M HCl with 3 vol% oxidants at 80℃ for 60 min. The ratio of hydrogen peroxide to sodium hypochlorite played a critical role in the leaching efficiency due to the supply of Cl- ions in the leachate. Moreover, the complete recovery of Pd in the leachate was achieved at 80℃ with 0.3 formic acid/leachate after adjusting the pH value of 7. This situation was ascribed to the decomposition of formic acid into hydrogen gas and carbon dioxide at 80℃. ICP-AES and XRD characterized the recovered Pd powder, and the purity of the recovered powder was found to be 99.6%. Consequently, the recovered Pd powder with high purity could be used in circuits, catalyst precursors, and surgical instruments.