• Journal of Powder Materials
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• v.28 no.5
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• pp.423-428
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• 2021

Here, we report the development of a new and low-cost core-shell structure for lithium-ion battery anodes using silicon waste sludge and the Ti-ion complex. X-ray diffraction (XRD) confirmed the raw waste silicon sludge powder to be pure silicon without other metal impurities and the particle size distribution is measured to be from 200 nm to 3 ㎛ by dynamic light scattering (DLS). As a result of pulverization by a planetary mill, the size of the single crystal according to the Scherrer formula is calculated to be 12.1 nm, but the average particle size of the agglomerate is measured to be 123.6 nm. A Si/TiO₂ core-shell structure is formed using simple Ti complex ions, and the ratio of TiO₂ peaks increased with an increase in the amount of Ti ions. Transmission electron microscopy (TEM) observations revealed that TiO₂ coating on Si nanoparticles results in a Si-TiO₂ core-shell structure. This result is expected to improve the stability and cycle of lithium-ion batteries as anodes.

• Journal of Powder Materials
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• v.28 no.4
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• pp.336-341
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• 2021

In this study, a nanocrystalline FeNiCrMoMnSiC alloy was fabricated, and its austenite stability, microstructure, and mechanical properties were investigated. A sintered FeNiCrMoMnSiC alloy sample with nanosized crystal was obtained by high-energy ball milling and spark plasma sintering. The sintering behavior was investigated by measuring the displacement according to the temperature of the sintered body. Through microstructural analysis, it was confirmed that a compact sintered body with few pores was produced, and cementite was formed. The stability of the austenite phase in the sintered samples was evaluated by X-ray diffraction analysis and electron backscatter diffraction. Results revealed a measured value of 51.6% and that the alloy had seven times more austenite stability than AISI 4340 wrought steel. The hardness of the sintered alloy was 60.4 HRC, which was up to 2.4 times higher than that of wrought steel.

• Journal of Powder Materials
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• v.28 no.3
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• pp.246-252
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• 2021

The effect of sintering conditions on the austenite stability and strain-induced martensitic transformation of nanocrystalline FeCrC alloy is investigated. Nanocrystalline FeCrC alloys are successfully fabricated by spark plasma sintering with an extremely short densification time to obtain the theoretical density value and prevent grain growth. The nanocrystallite size in the sintered alloys contributes to increased austenite stability. The phase fraction of the FeCrC sintered alloy before and after deformation according to the sintering holding time is measured using X-ray diffraction and electron backscatter diffraction analysis. During compressive deformation, the volume fraction of strain-induced martensite resulting from austenite decomposition is increased. The transformation kinetics of the strain-induced martensite is evaluated using an empirical equation considering the austenite stability factor. The hardness of the S0W and S10W samples increase to 62.4-67.5 and 58.9-63.4 HRC before and after deformation. The hardness results confirmed that the mechanical properties are improved owing to the effects of grain refinement and strain-induced martensitic transformation in the nanocrystalline FeCrC alloy.

• Korean Journal of Metals and Materials
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• v.49 no.4
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• pp.313-320
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• 2011

100 nm-thick hydrogenated amorphous silicon $({\alpha}-Si:H)$ films were deposited on a glass and glass/30 nm Ni substrates by inductively-coupled plasma chemical vapor deposition (ICP-CVD) at temperatures ranging from 100 to $550^{\circ}C$. The sheet resistance, microstructure, phase transformation and surface roughness of the films were characterized using a four-point probe, AFM (atomic force microscope), TEM (transmission electron microscope), AES (Auger electron spectroscopy), HR-XRD(high resolution X-ray diffraction), and micro-Raman spectroscopy. A nano-thick NiSi phase was formed at substrate temperatures >$400^{\circ}C$. AFM confirmed that the surface roughness did not change as the substrate temperature increased, but it increased abruptly to 6.6 nm above $400^{\circ}C$ on the glass/30 nm Ni substrates. HR-XRD and micro-Raman spectroscopy showed that all the Si samples were amorphous on the glass substrates, whereas crystalline silicon appeared at $550^{\circ}C$ on the glass/30 nm Ni substrates. These results show that crystalline NiSi and Si can be prepared simultaneously on Ni-inserted substrates.

• Korean Journal of Metals and Materials
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• v.46 no.4
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• pp.249-256
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• 2008

0.5 wt% Al doped ZnO thin films (AZO) were prepared on glass substrates using RF magnetron sputtering method. Thin films were grown at substrate temperature of $250^{\circ}C$, RF power of 75W, working pressure of 10 mTorr, by changing the $O_2/Ar$ pressure ratio from 0% to 16.7%. The effects of oxygen partial pressure during the deposition process on structural and optical properties of the films were investigated using XRD, SEM, AFM, EPMA and UV-visible spectroscopy. All the AZO thin films were grown as hexagonal wurtzite phase with the c-axis preferred out-of-plane orientation. The surface roughness and grain size of AZO films decreased with increasing oxygen ratio from 10.6 nm to 3.2 nm and 94.9 nm to 30.9 nm, respectively. On the other hand, the transmittance and band gap energy of the AZO films increased from 84.7% to 92.6% and 3.24 eV to 3.28 eV, respectively with increasing the $O_2/Ar$ pressure ratio.

• Korean Journal of Metals and Materials
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• v.46 no.2
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• pp.88-96
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• 2008

Thermal evaporated 10 nm-$Ni_{50}Co_{50}$/(70 nm-poly)Si films were deposited to examine the energy saving properties of silicides formed by rapid thermal annealing at temperature ranging from 500 to $1,100^{\circ}C$ for 40 seconds. Thermal evaporated 10 nm-Ni/(70 nm-poly)Si films were also deposited as a reference using the same method for depositing the 10 nm-$Ni_{50}Co_{50}$/(70 nm-poly)Si films. A four-point probe was used to examine the sheet resistance. Transmission electron microscopy (TEM) and X-ray diffraction XRD were used to determine cross sectional microstructure and phase changes, respectively. UV-VIS-NIR and FT-IR (Fourier transform infrared spectroscopy) were used to examine the near-infrared (NIR) and middle-infrared (MIR) absorbance. TEM analysis confirmed that the uniform nickel-cobalt composite silicide layers approximately 21 to 55 nm in thickness had formed on the single and polycrystalline silicon substrates as well as on the 25 to 100 nm thick nickel silicide layers. In particular, nickel-cobalt composite silicides showed a low sheet resistance, even after rapid annealing at $1,100^{\circ}C$. Nickel-cobalt composite silicide and nickel silicide films on the single silicon substrates showed similar absorbance in the near-IR region, while those on the polycrystalline silicon substrates showed excellent absorbance until the 1,750 nm region. Silicides on polycrystalline substrates showed high absorbance in the middle IR region. Nickel-cobalt composite silicides on the poly-Si substrates annealed at $1,000^{\circ}C$ superior IR absorption on both NIR and MIR region. These results suggest that the newly proposed $Ni_{50}Co_{50}$ composite silicides may be suitable for applications of IR absorption coatings.

• Korean Journal of Metals and Materials
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• v.49 no.6
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• pp.498-504
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• 2011

We examined the microstructure and optical properties of crystallized ~30 nm-ZnO/~10 nm amorphous $TiO_2$ nano bilayered films as nano electrodes were deposited at extremely low substrate temperatures of $150-210^{\circ}C$. The bilayered films were deposited on silicon substrates with 10 cm diameters by ALD (atomic layer deposition) using DEZn (diethyl zinc(Zn(C2H5)2)) and TDMAT (tetrakis dimethyl-amid $titanium(Ti(N(CH_3)_2)_4)$ as the ZnO and $TiO_2$ precursors, respectively, and $H_2O$ as the oxidant. The microstructure, phase, and optical properties of the bilayered films were examined by FE-SEM, TEM, XRD, AES, and UV-VIS-NIR spectroscopy. FE-SEM and TEM showed that all bilayered films were deposited very uniformly and showed crystallized ZnO and amorphous $TiO_2$ layers. AES depth profiling showed that the ZnO and $TiO_2$ films had a stoichiometric composition of 1:1 and 1:2, respectively. These bilayered films have optical absorption properties in a wide range of ultraviolet wavelengths, 250-390 nm, whereas the single ZnO and $TiO_2$ films showed an absorption range of 350-380nm.

• Korean Journal of Metals and Materials
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• v.48 no.2
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• pp.133-140
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• 2010

10 nm thick Ni layers were deposited on 200 nm $SiO_2/Si$ substrates using an e-beam evaporator. Then, 60 nm or 20 nm thick ${\alpha}$-Si:H layers were grown at low temperature (<$200^{\circ}C$) by a Catalytic-CVD. NiSi layers were already formed instantaneously during Cat-CVD process regardless of the thickness of the $\alpha$-Si. The resulting changes in sheet resistance, microstructure, phase, chemical composition, and surface roughness with the additional rapid thermal annealing up to $500^{\circ}C$ were examined using a four point probe, HRXRD, FE-SEM, TEM, AES, and SPM, respectively. The sheet resistance of the NiSi layer was 12${\Omega}$/□ regardless of the thickness of the ${\alpha}$-Si and kept stable even after the additional annealing process. The thickness of the NiSi layer was 30 nm with excellent uniformity and the surface roughness was maintained under 2 nm after the annealing. Accordingly, our result implies that the low temperature Cat-CVD process with proposed films stack sequence may have more advantages than the conventional CVD process for nano scale NiSi applications.

• Korean Journal of Metals and Materials
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• v.49 no.6
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• pp.505-513
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• 2011

A magnetic device which enables the application of a strong and uniform magnetic field to thin film during sputtering was designed for controlling the magnetic anisotropy using a three dimensional finite element method, and the effects of the external magnetic field on the magnetic properties of sputtered thin films were investigated. Both the intensity and the uniformity of the magnetic flux density in the sputter zone (50 mm ${\times}$50 mm) was dependent on not only the shape and size of the magnet device but also the magnitude of stray fields from the magnet. For the magnet device in which the distance between two magnets or two pure iron bars was 80-90 mm, the magnetic flux density along the direction normal to the external magnetic field direction was minimum. The two row magnets increased the magnetic flux density and uniformity along the external magnetic field direction. An Fe thin film sputtered using the optimized magnet device showed a higher remanence ratio than that fabricated under no external magnetic field.

• Korean Journal of Metals and Materials
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• v.49 no.4
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• pp.321-328
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• 2011

The 30 nm-thick Ni layers was deposited on a flexible polyimide substrate with an e-beam evaporation. Subsequently, we deposited a Si layer using a catalytic CVD (Cat-CVD) in a hydride amorphous silicon (${\alpha}$-Si:H) process of $T_{s}=180^{\circ}C$ with varying thicknesses of 55, 75, 145, and 220 nm. The sheet resistance, phase, degree of the crystallization, microstructure, composition, and surface roughness were measured by a four-point probe, HRXRD, micro-Raman spectroscopy, FE-SEM, TEM, AES, and SPM. We confirmed that our newly proposed Cat-CVD process simultaneously formed both NiSi and crystallized Si without additional annealing. The NiSi showed low sheet resistance of < $13{\Omega}$□, while carbon (C) diffused from the substrate led the resistance fluctuation with silicon deposition thickness. HRXRD and micro-Raman analysis also supported the existence of NiSi and crystallized (>66%) Si layers. TEM analysis showed uniform NiSi and silicon layers, and the thickness of the NiSi increased as Si deposition time increased. Based on the AES depth profiling, we confirmed that the carbon from the polyimide substrate diffused into the NiSi and Si layers during the Cat-CVD, which caused a pile-up of C at the interface. This carbon diffusion might lessen NiSi formation and increase the resistance of the NiSi.