• Journal of Sensor Science and Technology
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• v.25 no.3
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• pp.223-228
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• 2016

In this work, we prepared porous WO3 nanofibers (NFs) functionalized by bio-inspired catalytic $Cr_2O_3$ and $Co_3O_4$ nanoparticles as highly sensitive and selective $H_2S$ gas sensing layers. Highly porous 3-dimensional (3D) NFs networks decorated by well-dispersed catalyst NPs exhibited superior $H_2S$ gas response ($R_{air}/R_{gas}$ = 46 at 5 ppm) in high humidity environment (95 %RH). In particular, the sensors showed outstanding $H_2S$ selectivity against other interfering analytes (such as acetone, toluene, CO, $H_2$, ethanol). Exhaled breath sensors using $Cr_2O_3$ and $Co_3O_4$ catalysts-loaded $WO_3$ NFs are highly promising for the accurate detection of halitosis.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.198-198
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• 2015

전기변색재료는 전압을 인가하였을 때 전계방향에 따라 가역적으로 색이 변화하는 재료를 말한다. 스마트윈도우용 전기 변색재료는 지속적으로 전기를 가해줄 필요 없이 한번 변색되면 색이 지속되는 특징을 가지므로 에너지 효율적으로 우수하여 태양열 차단 창호나 디스플레이 분야에 응용될 것으로 기대된다. 이러한 전기 변색재료에는 산화형 전기 변색 재료, 환원형 전기 변색 재료가 있는데 이중 가장 널리 연구되고 있는 재료는 환원형 전기변색재료이다. 대표적인 재료로 $WO_3$가 쓰이는 데 이는 전기 변색적 특성이 우수하고 또한 내구성이 다른 재료에 비해 우수하다는 장점 때문이다. 그러나, 상용화를 위해서는 내구성의 개선이 요구되고 있다. 한편, $TiO_2$는 안정성이 매우 뛰어나지만 전기변색적 특성이 $WO_3$에 비해 낮은 점이 지적되고 있다. 이러한 $WO_3$ 및 $TiO_2$ 박막은 스퍼터링 또는 sol-gel법 등으로 제작되고 있는데, 일반적으로 스퍼터링의 경우 치밀한 박막이 형성되기 때문에 Porous 한 박막을 얻기 힘들다. 따라서 본 연구에서는 기판에 입사하는 스퍼터 입자들의 각도를 조절하여 shadowing 효과로 인해 박막의 구조가 porous해지는 Glancing angle deposition을 도입하였다. 이러한 증착법을 이용하여 $WO_3$와 $TiO_2$를 각도를 조절하여 증착하고 $TiO_2$와 $WO_3$ 박막의 특성을 비교하여 본다. 두께 300 nm를 가지는 $WO_3$ 및 $TiO_2$ 박막은 GLAD RF 마그네트론 스퍼터링법을 이용하여 Corning glass(corning E-2000)기판 위에 증착하였다. 기판 입사 각도는 $0^{\circ}$, $30^{\circ}$, $45^{\circ}$, $60^{\circ}$로 증착하였고 직경 3 in의 $TiO_2$, $WO_3$ 타겟을 사용하였다. 또한 스퍼터링 파워는 400 W, 작업압력 1.0 Pa, 그리고 스퍼터링 가스는 O2/Ar+O2 유량 10%에서 30%로 증착을 상온에서 진행하였다. 전기화학적 특성을 평가하기 위하여 $TiO_2$ 및 $WO_3$ 박막을 100 nm 두께의 ITO/glass 위에서 증착하였다. 박막의 미세구조는 XRD와 SEM을 통해 확인하였고, 전기화학적 특성은 Ar 분위기의 Glove box안에서 parstat 2273을 통해 측정하였다. 전해질은 1 M $LiPF_6/PC$로 진행하였고, 대향 전극는 Pt전극을, 참고 전극은 칼로멜 전극을 사용하였다. Potential 범위는 2 V에서 4 V로 진행하였고, scan rate는 50 mV/s로 측정하였다. 투과도는 UV/VIS spectrometer로 측정하였다. 전기변색 특성의 상관관계 및 에 대해서는 학회 당일 발표할 예정이다.

• Korean Journal of Materials Research
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• v.21 no.9
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• pp.520-524
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• 2011

Porous W with controlled pore characteristics was fabricated by a freeze-drying process. $WO_3$ powder and camphene were used as the source materials of W and sublimable vehicles, respectively. Camphene slurries with $WO_3$ contents of 10 and 15 vol% were prepared by milling at $50^{\circ}C$ with a small amount of oligomeric polyester dispersant. Freezing of a slurry was done in a Teflon cylinder attached to a copper bottom plate cooled at $-25^{\circ}C$ while the growth direction of the camphene was unidirectionally controlled. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was hydrogen-reduced at $800^{\circ}C$ for 30 min and sintered in a furnace at $900^{\circ}C$ for 1 h under a hydrogen atmosphere. Microstructural observation revealed that all of the sintered samples were composed of only W phase and showed large pores which were aligned parallel to the camphene growth direction. The porosity and pore size increased with increasing camphene content. The difference in the pore characteristics depending on the slurry concentration may be explained by the degree of powder rearrangement in the slurry. The results strongly suggest that a porous metal with the required pore characteristics can be successfully fabricated by a freeze-drying process using metal oxide powders.

• Journal of Sensor Science and Technology
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• v.29 no.1
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• pp.14-18
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• 2020

This study investigates the nitrogen dioxide (NO₂) sensing characteristics of an Si MOSFET gas sensor with a tungsten trioxide (WO₃) sensing layer deposited using the sputtering method. The Si MOSFET gas sensor consists of a horizontal floating gate (FG) interdigitated with a control gate (CG). The WO₃ sensing layer is deposited on the interdigitated CG-FG of a field effect transistor(FET)-type gas sensor platform. The sensing layer is deposited with different thicknesses of the film ranging from 100 nm to 1 ㎛ by changing the deposition times during the sputtering process. The sensing characteristics of the fabricated gas sensor are measured at different NO₂ concentrations and operating temperatures. The response of the gas sensor increases as the NO₂ concentration and operating temperature increase. However, the gas sensor has an optimal performance at 180℃ considering both response and recovery speed. The response of the gas sensor increases significantly from 24% to 138% as the thickness of the sensing layer increases from 100 nm to 1 ㎛. The sputtered WO₃ film consists of a dense part and a porous part. As reported in previous work, the area of the porous part of the film increases as the thickness of the film increases. This increased porous part promotes the reaction of the sensing layer with the NO₂ gas. Consequently, the response of the gas sensor increases as the thickness of the sputtered WO₃ film increases.

• Journal of Sensor Science and Technology
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• v.17 no.1
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• pp.9-14
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• 2008

In this paper, the gas responses of tungsten oxide films prepared by anodic reaction was discussed. Sensing electrodes and heating electrodes were patterned by photolithography method on quartz substrate. Porous tungsten oxide was fabricated in electrolyte solutions of 5 % HF (HF :$C_2H_6OH:H_2O$=3 : 2 : 20) by anodic reaction. The anodic reaction with metal (platinum wire) as a cathode and the sensing device as an anode was conducted under the various reaction times (1-10 min) at 10 mA/$cm^2$ The surface structure and morphology of the fabricated sensor have been analysed by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM). All the peaks of XRD results were well indexed to the pure phase pattern. The average diameter of the porous tungsten oxide surface were ranged about 100 nm. The fabricaed sensor showed good sensitivity to 200 ppm toluene at operating temperature of $250^{\circ}C$.

• Journal of Powder Materials
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• v.11 no.2
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• pp.111-117
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• 2004

The oxidation behavior of 91 WC-9Co hardmetal in weight percentage has been studied in the present work as a part of the development of recycling process. The morphological and compositional changes of the WC-Co hardmetal with oxidation time at 90$0^{\circ}C$ were analyzed by using surface observation and X-ray diffraction. respective]y. As the oxidation time increased, the WC-Co hardmetal was continuously expanded to form porous oxide mixtures of $CoWO_4$ and $WO_3$. The morphology of porous oxide mixture was basically dependent on initial shape of the WC-Co hardmetal. From thermo-gravimetric (TG) analysis, it was found that the oxidation rate was increased with increasing oxidation temperature and oxygen content in the flowing atmospheric gas. The fraction of oxidation versus time curves showed S-curve relationship at a given of oxidation temperature. These oxidation behaviors of the WC-Co hardmetal were discussed in terms of previously proposed kinetic models.

• Journal of Powder Materials
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• v.28 no.3
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• pp.216-220
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• 2021

The effect of tert-butyl alcohol (TBA) as a freezing solvent on the pore structure of a porous tungsten body prepared by freeze-drying is analyzed. TBA slurries with a WO3 content of 10 vol% are prepared by mixing with a small amount of dispersant and binder at 30℃. The slurries are frozen at -25℃, and pores are formed in the frozen specimens by the sublimation of TBA during drying in air. After hydrogen reduction at 800℃ and sintering at 1000℃, the green body of WO₃ is completely converted to porous W with various pore structures. Directional pores from the center of the specimen to the outside are observed in the sintered bodies because of the columnar growth of TBA. A decrease in pore directionality and porosity is observed in the specimens prepared by long-duration drying and sintering. The change in pore structure is explained by the growth of the freezing solvent and densification.

• 한국신재생에너지학회:학술대회논문집
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• 2011.11a
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• pp.99.2-99.2
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• 2011

Transparent conducting oxides (TCOs) supported on glass are widely used as substrates in PEC studies for photovoltaic hydrogen generation applications However, high sheet resistane ($10{\sim}15{\Omega}/cm^2$) and fragileness of glass-supported TCO substrates are the obstacles to produce the large area PEC cells. Such internal sheet resistance is detrimental to efficient collection of photogenerated majority charge carriers at the photoactive material and electrolyte interface. Moreover, these TCO substrates are very expensive and consume about 40~60% cost of the devices. Hence, a low sheet resistance of the substrate is a key point in improving the performance of PEC devices. Metallic substrates coated with a photoactive material would be a good choice for efficient charge collection. Such metal substrates based photanodes are best candidate for large-scale phtoelectrochemical water splitting for hydrogen generation. In this study, we report the enhanced PEC performance of $WO_3$ film on metal(chemical etched, bare) substrate. It is proposed that interface between $WO_3$ and the metal substrate is responsible for efficient charge transfer and demonstrated significant improvement in the photoelectrochmical performance. X-ray diffration and FESEM suduies reveled that $WO_3$ films are monoclinic, porous, polycrystalline with average grain size of ~50nm. Photocurrent of $WO_3$ prepared on metal substrates was measured in 0.5M $H_2SO_4$ electroyte under simulated $100mW/cm^2$ illumination.

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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• pp.25.2-25.2
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• 2011

The tungsten oxide wire-like nanostructure is fabricated by deposition and thermal oxidation of tungsten metal on porous single wall carbon nanotubes (SWNTs). The morphology and crystalline quality of materials are investigated by SEM, TEM, XRD and Raman analysis. The results prove that $WO_3$ wire-like nanostructure fabricated on SWNTs show highly porous structures. Exposure of the sensors to NH3 gas in the temperature range of 150~300$^{\circ}C$ resulted in the highest sensitivity at $250^{\circ}C$ with quite rapid response and recovery time. Response time as a function of test concentrations and NH3 gas sensing mechanism is reported and discussed.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.115.1-115.1
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• 2016

Electrochemical anodization has been interested due to its useful way for the nano-scale architecture of metal oxides obtained from a metal substrate. By using this method, it is easy to control the morphology of the oxide materials by controlling electrochemical conditions. Among oxide materials obtained from the transition metals such as Ti, V, W, etc., in this paper, the morphological study of anodized $TiO_2$ was employed at various voltage conditions in fluoric based electrolyte, and the effects of applied voltage (sweep rate and retention time) on the tube morphologies were investigated. Furthermore, by using anodization of tungsten substrate (W), we fabricated the porous structure of $WO_3$ and provided merits of tailored structure for the hybridization of inorganic and organic materials as electrochromic (EC) applications. The hybrid porous $WO_3$ shows multi-chromic properties during the EC reactions at specific voltage conditions. From these results, the anodization process with tailoring nano-structure is one of the promising methods for EC applications.