• Title/Summary/Keyword: TEM microstructure

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Synthesis of MnO2 Nanowires by Hydrothermal Method and their Electrochemical Characteristics (수열합성법을 이용한 망간 나노와이어 제조 및 이의 전기화학적 특성 연구)

  • Hong, Seok Bok;Kang, On Yu;Hwang, Sung Yeon;Heo, Young Min;Kim, Jung Won;Choi, Bong Gill
    • Applied Chemistry for Engineering
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    • v.27 no.6
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    • pp.653-658
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    • 2016
  • In this work, we developed a synthetic method for preparing one-dimensional $MnO_2$ nanowires through a hydrothermal method using a mixture of $KMnO_4$ and $MnSO_4$ precursors. As-prepared $MnO_2$ nanowires had a high surface area and porous structure, which are beneficial to the fast electron and ion transfer during electrochemical reaction. The microstructure and chemical structure of $MnO_2$ nanowires were characterized by scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and Brunauer-Emmett-Teller measurements. The electrochemical properties of $MnO_2$ nanowire electrodes were also investigated using cyclic voltammetry and galvanostatic charge-discharge with a three-electrode system. $MnO_2$ nanowire electrodes showed a high specific capacitance of 129 F/g, a high rate capability of 61% retention, and an excellent cycle life of 100% during 1000 cycles.

A Study on the Change of Microstructures by Heat-treatment in Mo-Hf-C Alloys (Mo-Hf-C계 합금의 열처리에 따른 미세조직 변화에 관한 연구)

  • Yoon, Kook-Han;Kim, Hyeong-Ki;Lee, Chong-Mu;Park, Won-Koo;Choi, Ju
    • Korean Journal of Materials Research
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    • v.3 no.2
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    • pp.111-120
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    • 1993
  • Abstract In this study, the Mo-Hf-O ingots containing 0.31-1.14at % Hf and 0.08-1.00at % 0 were prepared by plasma arc melting. The change of microstructure depending on the condition of heat treatmen~ was analysed by optical microscophy, auger electron microscophy, and transmission electron microscophy. Molybdenum powder with the oxygen content of 830ppm was compacted, and then melted. The oxygen content of molybdenum ingots was detected to be 40 -130ppm. As the contents of Hf and 0 increased, the grain size of ingots decreased. When molybdenum igot containing l.14at % Hf and 1.00at % C was heat treated, p-molybdenum carbide in grains was transformed into ${\alpha}$-molybdenum carbide at 130$0^{\circ}C$. Between 140$0^{\circ}C$ and 150$0^{\circ}C$, the precipitation of hafnium carbide was due to the reaction of solute Hf and C, and the hafnium carbide was saturated at grain boundaries at 150$0^{\circ}C$. When the sample was heat treated from 150$0^{\circ}C$ to 170$0^{\circ}C$, Hafnium oxide more stable thermodynamically precipitated both at grain boundaries and in grains after hafnium carbide had been dissolved at grain boundaries.

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The Effect of Carbide Precipitation on the High Temperature Deformation of Ni3Al and TiAl

  • Han, Chang-Suk;Kim, Jang-Woo;Kim, Young-Woo
    • Korean Journal of Metals and Materials
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    • v.47 no.3
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    • pp.147-154
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    • 2009
  • The effect of carbon addition on the microstructures and mechanical properties of $Ni_3Al$ and TiAl intermetallic alloys have been characterized. It is shown that carbon is not only an efficient solid solution strengthener in $Ni_3Al$ and TiAl, it is also an efficient precipitation strengthener by fine dispersion of carbide. Transmission electron microscope investigation has been performed on the particle-dislocation interactions in $Ni_3Al$ and TiAl intermetallics containing various types of fine precipitates. In an $L1_2$-ordered $Ni_3Al$ alloy with 4 mol.% of chromium and 0.2~3.0 mol.% of carbon, fine octahedral precipitates of $M_{23}C_6$ type carbide, which has the cube-cube orientation relationship with the matrix, appear during aging. Typical Orowan loops are formed in $Ni_3Al$ containing fine dispersions of $M_{23}C_6$ particles. In the L10-ordered TiAl containing 0.1~2.0 mol.% carbon, TEM observations revealed that needle-like precipitates, which lie only in one direction parallel to the [001] axis of the $L1_0$ matrix, appear in the matrix and preferentially at dislocations. Selected area electron diffraction (SAED) patterns analyses have shown that the needle-shaped precipitate is $Ti_3AlC$ of perovskite type. The orientation relationship between the $Ti_3AlC$ and the $L1_0$ matrix is found to be $(001)_{Ti3AlC}//(001)_{L10\;matrix}$ and $[010]_{Ti3AlC}//[010]_{L10\;matrix}$. By aging at higher temperatures or for longer period at 1073 K, plate-like precipitates of $Ti_2AlC$ with a hexagonal structure are formed on the {111} planes of the $L1_0$ matrix. The orientation relationship between the $(0001)_{Ti2AlC}//(111)_{L10\;matrix}$ is and $[1120]_{Ti2AlC}//[101]_{L10\;matrix}$. High temperature strength of TiAl increases appreciably by the precipitation of fine carbide. Dislocations bypass the carbide needles at further higher temperatures.

Property of Nickel Silicides with 10 nm-thick Ni/Amorphous Silicon Layers using Low Temperature Process (10 nm-Ni 층과 비정질 실리콘층으로 제조된 저온공정 나노급 니켈실리사이드의 물성 변화)

  • Choi, Youngyoun;Park, Jongsung;Song, Ohsung
    • Korean Journal of Metals and Materials
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    • v.47 no.5
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    • pp.322-329
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    • 2009
  • 60 nm- and 20 nm-thick hydrogenated amorphous silicon (a-Si:H) layers were deposited on 200 nm $SiO_2/Si$ substrates using ICP-CVD (inductively coupled plasma chemical vapor deposition). A 10 nm-Ni layer was then deposited by e-beam evaporation. Finally, 10 nm-Ni/60 nm a-Si:H/200 nm-$SiO_2/Si$ and 10 nm-Ni/20 nm a-Si:H/200 nm-$SiO_2/Si$ structures were prepared. The samples were annealed by rapid thermal annealing for 40 seconds at $200{\sim}500^{\circ}C$ to produce $NiSi_x$. The resulting changes in sheet resistance, microstructure, phase, chemical composition and surface roughness were examined. The nickel silicide on a 60 nm a-Si:H substrate showed a low sheet resistance at T (temperatures) >$450^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate showed a low sheet resistance at T > $300^{\circ}C$. HRXRD analysis revealed a phase transformation of the nickel silicide on a 60 nm a-Si:H substrate (${\delta}-Ni_2Si{\rightarrow}{\zeta}-Ni_2Si{\rightarrow}(NiSi+{\zeta}-Ni_2Si)$) at annealing temperatures of $300^{\circ}C{\rightarrow}400^{\circ}C{\rightarrow}500^{\circ}C$. The nickel silicide on the 20 nm a-Si:H substrate had a composition of ${\delta}-Ni_2Si$ with no secondary phases. Through FE-SEM and TEM analysis, the nickel silicide layer on the 60 nm a-Si:H substrate showed a 60 nm-thick silicide layer with a columnar shape, which contained both residual a-Si:H and $Ni_2Si$ layers, regardless of annealing temperatures. The nickel silicide on the 20 nm a-Si:H substrate had a uniform thickness of 40 nm with a columnar shape and no residual silicon. SPM analysis shows that the surface roughness was < 1.8 nm regardless of the a-Si:H-thickness. It was confirmed that the low temperature silicide process using a 20 nm a-Si:H substrate is more suitable for thin film transistor (TFT) active layer applications.

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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