• Title/Summary/Keyword: XRD Analysis

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Analysis of Photovoltaic Performance Improvement of Cu2Zn1-xCdxSn(SxSe1-x)4 Thin Film Solar Cells by Controlling Cd2+ Element Alloying Time Using CBD Method (CBD 공법을 이용하여 Cd2+ 원소 Alloying 시간을 조절한 Cu2Zn1-xCdxSn(SxSe1-x)4 박막 태양전지의 광전지 성능 향상 분석)

  • Sang Woo, Park;Suyoung, Jang;Jun Sung, Jang;Jin Hyeok, Kim
    • Korean Journal of Materials Research
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    • v.32 no.11
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    • pp.481-488
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    • 2022
  • The Cu2ZnSn(SxSe1-x)4 (CZTSSe) absorbers are promising thin film solar cells (TFSCs) materials, to replace existing Cu(In,Ga)Se2 (CIGS) and CdTe photovoltaic technology. However, the best reported efficiency for a CZTSSe device, of 13.6 %, is still too low for commercial use. Recently, partially replacing the Zn2+ element with a Cd2+element has attracting attention as one of the promising strategies for improving the photovoltaic characteristics of the CZTSSe TFSCs. Cd2+ elements are known to improve the grain size of the CZTSSe absorber thin films and improve optoelectronic properties by suppressing potential defects, causing short-circuit current (Jsc) loss. In this study, the structural, compositional, and morphological characteristics of CZTSSe and CZCTSSe thin films were investigated using X-ray diffraction (XRD), X-ray fluorescence spectrometer (XRF), and Field-emission scanning electron microscopy (FE-SEM), respectively. The FE-SEM images revealed that the grain size improved with increasing Cd2+ alloying in the CZTSSe thin films. Moreover, there was a slight decrease in small grain distribution as well as voids near the CZTSSe/Mo interface after Cd2+ alloying. The solar cells prepared using the most promising CZTSSe absorber thin films with Cd2+ alloying (8 min. 30 sec.) exhibited a power conversion efficiency (PCE) of 9.33 %, Jsc of 34.0 mA/cm2, and fill factor (FF) of 62.7 %, respectively.

Phase evaluation of Fe/Co pigments coated porcelain by rietveld refinement (리트벨트 정밀화법에 의한 Fe/Co 안료가 코팅된 도자기의 상분석)

  • Nam-Heun Kim;Kyung-Nam Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.33 no.5
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    • pp.174-180
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    • 2023
  • Porcelain (white ware, celadon ware) coated with a ferrous sulfate and ferrous/cobalt sulfate was sintered at 1250℃. The specimens were investigated by HR-XRD, FE-SEM, HR-EDS, and UV-vis spectrophotometer. Through X-ray rietveld quantitative analysis, quartz and mullite were found to be the main phases for white ware, and mullite and plagioclase were found to be the main phases for celadon ware. When the pigment of ferrous/cobalt sulfate was applied, were identified as an andradite phase for celadon ware and a spinel phase for the white ware, and the amorphous phase, respectively. The L* value, which was the brightness of the specimen, was 72.01, 60.92 for white ware and celadon ware, respectively. The ferrous and ferrous/cobalt pigment coated porcelain had L* values of 44.89, 52.27 for white ware and celadon ware, respectively; with a* values of 2.12, 1.40, an d at b* values of 1.45 and 13.79. As for the color of the specimens, it was found that the L* value was greatly affected by the white ware, and the b* value differed greatly depending on the clay. It was thought to be closely related to the production of the secondary phase such as Fe2O3 and andradite phase produced in the surface layer.

Materialistic Characterization of Waste Egg Shell and Fundamental Studies for Its Application to Wastewater Treatment (폐달걀껍질의 활용을 위한 물성조사 및 폐수처리 응용에의 기초연구)

  • Kuh, Sung-Eun;Kim, Dong-Su
    • Journal of Korean Society of Environmental Engineers
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    • v.22 no.4
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    • pp.733-742
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    • 2000
  • Fundamental materialistic characterization and adsorption/neutralization behavior of waste egg shell for heavy metal ion have been studied for its application to wastewater treatment. To investigate the structural change and thermal decomposition characteristics of egg shell. X-ray diffraction and FT-IR analysis were conducted for egg shell treated at $105^{\circ}C$ and $700^{\circ}C$, respectively. For the result of FT-IR analysis, the sample treated at $700^{\circ}C$ showed a reduced C-O absorption band compared with that of egg shell treated at $105^{\circ}C$, which may be due to the $CO_2$ release. Unlike to the result of FT-IR analysis, the XRD patterns of egg shell were almost similar for the cases of $105^{\circ}C$ and $700^{\circ}C$ treatment. however, characteristic diffraction pattern of CaO was observed for $850^{\circ}C$ treatment, at which $CaCO_3$ is known to be completely converted to CaO. TGA/DTA analysis showed a slow decline in weight loss up to $600^{\circ}C$ and, for $600{\sim}800^{\circ}C$ range, the weight loss became drastic by reason of $CO_2$ discharge, which was accompanied by an appearance of major endothermic peak. The ratio of practical breakthrough time to ideal one, total transfer unit, and mass transfer coefficient were observed to be increased as the adsorption was progressed in a multiple-column fixed-bed reactor using egg shell as an adsorbent, which signified the distribution effect of mass transfer for continuous adsorption reaction. The neutralization effect of egg shell for several types of acidic wastewater made of different mineral acids was not much different from each other except for the case of $H_2SO_4$, for which the neutralization reaction was thought to be retarded by the formation of gypsum.

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Comparative Analysis of Heavy Metal Contamination, Mineral Composition and Spectral Characteristics of White, Reddish Brown and Mixed Precipitates Occurring at Osip Stream Drainage, Gangwondo, South Korea (강원도 오십천 수계에 분포하는 백색침전물, 적갈색침전물 및 혼합침전물의 중금속 오염, 광물조성 및 분광학적 특성의 비교분석)

  • Lim, Jeong Hwa;Yu, Jaehyung;Shin, Ji Hye;Koh, Sang-Mo
    • Economic and Environmental Geology
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    • v.52 no.1
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    • pp.13-28
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    • 2019
  • This study analyzed precipitation environment, heavy metal contamination, and mineral composition of white, reddish brown and mixed precipitates occurring at the Osip stream drainage, Gangwondo. Furthermore, spectral characteristics of the precipitates associated with heavy metal contamination and mineral composition was investigated based on spectroscopic analysis. The pH range of the precipitates was 4.43-6.91 for white precipitates, 7.74-7.94 for reddish brown precipitates, and 7.59-7.9 for the mixed precipitates, respectively. XRF analysis revealed that these precipitates were contaminated with Ni, Cu, Zn, and As. The white precipitates showed high Al concentration compared to reddish brown precipitates as much as 3.3 times, and the reddish brown precipitates showed high Fe concentration compared to white precipitates as much as 15 times. XRD analysis identified that the mineral composition of the white participates was aluminocoquimbite, gibbsite, quartz, saponite, and illite, and that of reddish brown precipitates was aluminum isopropoxide, kaolinite, goethite, dolomite, pyrophyllite, magnetite, quartz, calcite, pyrope. The mineral composition of the mixed precipitates was quartz, albite, and calcite. The spectral characteristics of the precipitates was manifested by gibbsite, saponite, illite for white precipitates, goethite, kaolinite, pyrophyllite for reddish brown precipitates, and albite for the mixed precipitates, respectively. The spectral reflectance of the precipitates decreased with increase in heavy metal contamination, and absorption depth of the precipitates indicated that the heavy metal ions were adsorbed to saponite and illite for white precipitates, and goethite and magnetite for reddish brown precipitates.

Mineralogical Analysis of Calcium Silicate Cement according to the Mixing Rate of Waste Concrete Powder (폐콘크리트 미분말 치환율에 따른 이산화탄소 반응경화 시멘트의 광물상 분석)

  • Lee, Hyang-Sun;Song, Hun
    • Journal of the Korea Institute of Building Construction
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    • v.24 no.2
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    • pp.181-191
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    • 2024
  • In the realm of cement manufacturing, concerted efforts are underway to mitigate the emission of greenhouse gases. A significant portion, approximately 60%, of these emissions during the cement clinker sintering process is attributed to the decarbonation of limestone, which serves as a fundamental ingredient in cement production. Prompted by these environmental concerns, there is an active pursuit of alternative technologies and admixtures for cement that can substitute for limestone. Concurrently, initiatives are being explored to harness technology within the cement industry for the capture of carbon dioxide from industrial emissions, facilitating its conversion into carbonate minerals via chemical processes. Parallel to these technological advances, economic growth has precipitated a surge in construction activities, culminating in a steady escalation of construction waste, notably waste concrete. This study is anchored in the innovative production of calcium silicate cement clinkers, utilizing finely powdered waste concrete, followed by a thorough analysis of their mineral phases. Through X-ray diffraction(XRD) analysis, it was observed that increasing the substitution level of waste concrete powder and the molar ratio of SiO2 to (CaO+SiO2) leads to a decrease in Belite and γ-Belite, whereas minerals associated with carbonation, such as wollastonite and rankinite, exhibited an upsurge. Furthermore, the formation of gehlenite in cement clinkers, especially at higher substitution levels of waste concrete powder and the aforementioned molar ratio, is attributed to a synthetic reaction with Al2O3 present in the waste concrete powder. Analysis of free-CaO content revealed a decrement with increasing substitution rate of waste concrete powder and the molar ratio of SiO2/(CaO+SiO2). The outcomes of this study substantiate the viability of fabricating calcium silicate cement clinkers employing waste concrete powder.

Pedological and Mineralogical Characterizations of Hwangto (Yellow Residual Soils), Naju, Jeollanam-do, Korea (전라남도 나주시 동강면 일대 황토(풍화잔류토)의 토양학적 및 광물학적 특성 연구)

  • Kim, Yumi;Bae, Jo-Ri;Kim, Cheong-Bin;Roh, Yul
    • Economic and Environmental Geology
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    • v.47 no.2
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    • pp.87-96
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    • 2014
  • The objectives of this study were to characterize the physicochemical properties and mineralogy of Hwangto (yellow residual soils) from the southwestern part of Korea and to understand the soil-forming processes of the residual soils from their parent rocks. Both the yellowish residual soils as well as the unweathered and weathered parent rocks were obtained from Jangdong-ri, Donggang-myun, Naju, Jeollanam-do, Korea. The soil samples were examined to analyze the said soil's physicochemical properties such as color, pH, and particle size distribution. A scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM) and X-ray diffraction (XRD) analysis were performed in order to understand the mineralogy, chemical composition, and morphology of the soils. Two thin sections of a parent rock were analyzed to study its mineral composition. A particle size analysis of the soils indicates that the residual soil consists of mainly silt and clay (approximately 95%) and that soil textures are silty clay or silt clay loam. The soil colors of the residual soil are dark brown (7.5YR 3/4) through yellowish red (5YR 4/6). The pH of the residual soil ranges from 4.3 to 5.1. The major minerals of the parent rocks were quartz, biotite, chlorite, and plagioclase. The mineralogy of the sand fraction of the residual soil was quartz, biotite, muscovite and sanidine. The mineralogy of the silt fraction of the residual soil was quartz, biotite, muscovite, Na-feldspar, K-feldspar, and sanidine. The clay mineralogy of the soil was goethite, kaolinite, ilite, hydroxy-interlayed vermiculite(HIV), vermiculite, mica, K-feldspar and quartz. The mineral composition of the residual soil and the parent rock indicates that feldspar and mica in the parent rock weathered into illite, vermiculite and hydroxy-interlayed vermiculite(HIV), and finally changed into kaolinite and halloysite in the yellowish residual soils.

Mineralogy and Biogeochemistry of Intertidal Flat Sediment, Muan, Chonnam, Korea (전남 무안 갯벌 퇴적물에 관한 광물학적 및 생지화학적 연구)

  • Park, Byung-No;Lee, Je-Hyun;Oh, Jong-Min;Lee, Seuug-Hee;Han, Ji-Hee;Kim, Yu-Mi;Seo, Hyun-Hee;Roh, Yul
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.1 s.51
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    • pp.47-60
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    • 2007
  • While sedimentological researches on Western coastal tidal flats of Korea have been much pelformed previously, mineralogical and biogeochemical studies are beginning to be studied. The objectives of this study were to investigate mineralogical characteritics of the inter-tidal flat sediments and to explore phase transformation of iron(oxyhydr)oxides and biomineralization by metal-reducing bacteria enriched from the inter-tidal flat sediments from Muan, Jeollanam-do, Korea. Inter-tidal flat sediment samples were collected in Chungkye-myun and Haeje-myun, Muan-gun, Jeollanam-do. Particle size analyses were performed using the pipette method and sedimentation method. The separates including sand, silt and clay fractions were examined by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, transmission electron microscopy (TEM), and X-ray diffiaction (XRD). After enriching the metal-.educing bacteria from the into,-tidal flat sediments, the bacteria were used to study phase transformation of the synthesized iron (oxyhydr)oxides and iron biomineralization using lactate or glucose as the electron donors and Fe(III)-containing iron oxides as the electron accepters. Mineralogical studies showed that the sediments of tidal flats in Chung]rye-myun and Haeje-myun consist of quartz, plagioclase, microcline, biotite, kaolinite and illite. Biogeochemical researches showed that the metal-reducing bacteria enriched from the inter-tidal flat sediments reduced reddish brown akaganeite and mineralized nanometer-sized black magnetite. The bacteria also reduced the reddish brown ferrihydrite into black amorphous phases and reduced the yellowish goethite into greenish with formation of nm-sized phases. These results indicate that microbial Fe(III) reduction may play one of important roles in iron and carbon biogeochemistry as well as iron biomineralization in subsurface environments.

Research of Diffusion Bonding of Tungsten/Copper and Their Properties under High Heat Flux

  • Li, Jun;Yang, Jianfeng
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.14-14
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    • 2011
  • W (tungsten)-alloys will be the most promising plasma facing armor materials in highly loaded plasma interactive components of the next step fusion reactors due to its high melting point, high sputtering resistance and low deuterium/tritium retention. The bonding technology of tungsten to Cu alloy was one of the key issues. In this paper, W/CuCrZr diffusion bonding has been performed successfully by inserting pure metal interlay. The joint microstructure, interfacial elements migration and phase composition were analyzed by SEM, EDS, XRD, and the joint shear strength and micro-hardness were investigated. The mock-ups were fabricated successfully with diffusion bonding and the cladding technology respectively, and the high heat flux test and thermal fatigue test were carried out under actively cooling condition. When Ni foil was used for the bonding of tungsten to CuCrZr, two reaction layers, Ni4W and Ni(W) layer, appeared between the tungsten and Ni interlayer with the optimized condition. Even though Ni4W is hard and brittle, and the strength of the joint was oppositely increased (217 MPa) due primarily to extremely small thicknesses (2~3 ${\mu}m$). When Ti foil was selected as the interlayer, the Ti foil diffused quickly with Cu and was transformed into liquid phase at $1,000^{\circ}C$. Almost all of the liquid was extruded out of the interface zone under bonding pressure, and an extremely thin residual layer (1~2 ${\mu}m$) of the liquid phase was retained between the tungsten and CuCrZr, which shear strength exceeded 160 MPa. When Ni/Ti/Ni multiple interlayers were used for bonding of tungsten to CuCrZr, a large number of intermetallic compound ($Ni_4W/NiTi_2/NiTi/Ni_3T$) were formed for the interdiffusion among W, Ni and Ti. Therefore, the shear strength of the joint was low and just about 85 MPa. The residual stresses in the clad samples with flat, arc, rectangle and trapezoid interface were estimated by Finite Element Analysis. The simulation results show that the flat clad sample was subjected maximum residual stress at the edge of the interface, which could be cracked at the edge and propagated along the interface. As for the rectangle and trapezoid interface, the residual stresses of the interface were lower than that of the flat interface, and the interface of the arc clad sample have lowest residual stress and all of the residual stress with arc interface were divided into different grooved zones, so the probabilities of cracking and propagation were lower than other interfaces. The residual stresses of the mock-ups under high heat flux of 10 $MW/m^2$ were estimated by Finite Element Analysis. The tungsten of the flat interfaces was subjected to tensile stresses (positive $S_x$), and the CuCrZr was subjected to compressive stresses (negative $S_x$). If the interface have a little microcrack, the tungsten of joint was more liable to propagate than the CuCrZr due to the brittle of the tungsten. However, when the flat interface was substituted by arc interfaces, the periodical residual stresses in the joining region were either released or formed a stress field prohibiting the growth or nucleation of the interfacial cracks. Thermal fatigue tests were performed on the mock-ups of flat and arc interface under the heat flux of 10 $MW/m^2$ with the cooling water velocity of 10 m/s. After thermal cycle experiments, a large number of microcracks appeared at the tungsten substrate due to large radial tensile stress on the flat mock-up. The defects would largely affect the heat transfer capability and the structure reliability of the mock-up. As for the arc mock-up, even though some microcracks were found at the interface of the regions, all microcracks with arc interface were divided into different arc-grooved zones, so the propagation of microcracks is difficult.

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A Conversion of AFm Phases by Addition of CaCO3, CaCl2 and CaSO4 · 2H2O (CaCO3, CaCl2 및 CaSO4 · 2H2O 첨가에 의한 AFm상의 변화)

  • 이종규;추용식
    • Journal of the Korean Ceramic Society
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    • v.40 no.1
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    • pp.24-30
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    • 2003
  • A formation and conversion of AFm phases decisively play role in the hydration, hardening and corrosion processes of various cement. In this study, the conversion of Alumino-Ferrite Monohydrates(AFm) phases under the addition of $CaCO_3,;CaCl_2;and;CaSO_4{cdot}2H_2O$was investigated by the XRD quantitative analysis. The thypical AFm phases are $M_S(monosulfoaluminate),;M_C(monocarboaluminate);and;M_{Cl}(monochloroaluminate and also Called Friedel's salts)$in this cementitious system, The conversion reaction were not occurred in $M_C-CaCO_3,;M_{Cl}-CaCO_3$ and $M_{Cl}-CaCl_2$system. However, in $M_S-CaCO_3$ system, ettringite and $monocarboaluminate(M_C)$ were formed. In $M_S-CaCl_2;system;M_S$ was transformed to Friedel's $salts(M_{Cl})$ and ettringite was formed. In the case of $CaSO_4{cdot}2H_2O$ addition, all AFm $phases(M_S,;M_C;and;M_{Cl})$ were transformed to ettringite. The order of stabilization of AFm phases under $CaCO_3,;CaCl_2;and;CaSO_4{cdot}2H_2O$ was as follows : $M_S< M_C

A bilayer diffusion barrier of atomic layer deposited (ALD)-Ru/ALD-TaCN for direct plating of Cu

  • Kim, Soo-Hyun;Yim, Sung-Soo;Lee, Do-Joong;Kim, Ki-Su;Kim, Hyun-Mi;Kim, Ki-Bum;Sohn, Hyun-Chul
    • 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.

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