아연(zinc) 분말은 철의 부식을 막아주는 희생양극의 기능으로 자동차, 선박 및 철구조물의 부식을 방지하 는데 널리 사용되고 있다. 그러나 아연 분말은 높은 비중 때문에 수지나 용매 내에서 분산성이 저하되고 빠르게 침전이 일어나는 단점을 가진다. 본 연구에서는 실리카(SiOx)를 미세 아연분말의 표면에 코팅함으로써 아연분말의 물성 및 기능을 개선하고자 하였다. 아연분말의 실리카 표면코팅은 졸-겔법을 사용하였고 SEM/EDS의 표면 및 성분분석과 TEM 단면분석을 통하여 불순물이 잔존하지 않는 실리카 코팅이 성공적으로 형성됨과 그 코팅의 두께를 확인 할 수 있었다. 한편 코팅공정의 반복회수와 평균입도 변화와의 관계를 측정하여 2회까지의 반복코팅이 분산안정성을 유지하는데 효과적임을 확인하였다. 이 밖에 실리카 코팅 아연분말의 진비중(true density) 측정을 통해 코팅 공정에 의해 비중이 20% 이상 감소함을 확인하였고 제타포텐셜 측정으로 실리카 코팅에 의해 아연분말의 분산안정성이 4배까지 증가함을 확인하였다. 마지막으로 질산수용액 담지를 통해 실리카 코팅 아연분말의 내산성 향상 또한 확인하였다. 따라서 본 연구에서 제조된 실리카 코팅 아연분말은 방청 안료의 원료로 적합할 것으로 기대된다.
본 연구에서는 투명도와 기계적 특성을 향상시키기 위해 저온 공정의 졸-겔 법을 이용하여 하이브리드 복합체의 코팅 박막을 제조하였다. 하이브리드 복합체로는 ZrO2/TiO2/organosilane을 사용하였으며, 그 중 organosilane은 3-(trimethoxysilyl)propyl methacrylate을 사용하였고 이는 저온 공정의 광경 화 반응을 위해 도입되었다. 다양한 조성비로 합성된 복합체를 폴리 카보네이트 기판 위에 저온 공정의 졸 -겔 법을 이용하여 광경화와 열처리 공정을 거처 코팅 박막을 제조하였고 이 코팅 박막의 광학 특성 및 기계적 강도를 확인하였다. 코팅 박막은 가시광선 영역에서 97.5 % 이상의 투과도를 가짐을 확인하였고 기계적 강도는 9H 이상의 연필 경도를 가진 것을 확인하였다. 특히 ZTS-2-1 코팅 박막의 나노 압입 경도는 1.14 GPa로 가장 높게 측정되었다.
Cost-effective functional phosphor nanoparticles are prepared by introducing low-cost SiO2 spheres to rareearth phosphor (YVO4:Eu3+, YVO4:Er3+, and YVO4:Nd3+) shells using a sol-gel synthetic method. These functional nanoparticles are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy, and general photoluminescence spectra. The SiO2 sphere occupying the interior of the conventional phosphor is advantageous in significantly reducing the cost of expensive rare-earth phosphor nanoparticles. The sol-gel process facilitates the core–shell structure formation; the rare-earth shell phosphor has strong interactions with chelating agents on the surfaces of SiO2 nanoparticles and thus forms layers of several nanometers in thickness. The photoluminescence wavelength is simply tuned by replacing the active materials of Eu3+, Er3+, and Nd3+. Moreover, the photoluminescent properties of the core–shell nanoparticles can be optimized by manipulating the specific contents of active materials in the phosphors. Our simple approach substitutes low-cost SiO2 for expensive rare-earth-based phosphor materials to realize cost-effective phosphor nanoparticles for various applications.
Ho3+/Yb3+/Tm3+ tri-doped NaY1-x(WO4)2 phosphors with proper doping concentrations of Ho3+, Yb3+ and Tm3+ (x = Ho3+ +Yb3+ +Tm3+, Ho3+ = 0.04, 0.03, 0.02, 0.01, Yb3+ = 0.35, 0.40, 0.45, 0.50 and Tm3+ = 0.01, 0.02, 0.03, 0.04) were successfully synthesized via the microwave sol-gel route, and their upconversion properties were investigated. Well-crystallized microcrystalline particles showed fine and homogeneous microcrystalline morphology with particle sizes of 1-2 μm. The optical properties were comparatively examined using photoluminescence emission and Raman spectroscopy. Under excitation at 980 nm, the doped particles exhibited white emissions based on blue, green and red emission bands, which correspond to the 1G4→ 3H6 transitions of Tm3+ in the blue region, the 5S2/ 5F4→ 5I8 transitions of Ho3+ in the green region, the 5F5→ 5I8 transitions of Ho3+, and the 1G4→ 3F4 and 3H4→ 3H6 transitions of Tm3+ in the red region. The pump power dependence of the upconversion emission intensity and the Commission Internationale de L'Eclairage chromaticity coordinates of the phosphors were evaluated in detail.
TiO2 nanoparticles were synthesized by a sol-gel process using titanium tetra isopropoxide as a precursor at room temperature. Ag-doped TiO2 nanoparticles were prepared by photoreduction of AgNO3 on TiO2 under UV light irradiation and calcinated at 400 oC. Ag-doped TiO2 nanoparticles were characterized for their structural and morphological properties by Xray diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and transmission electron microscopy (TEM). The photocatalytic properties of the TiO2 and Ag-doped TiO2 nanoparticles were evaluated according to the degree of photocatalytic degradation of gaseous benzene under UV and visible light irradiation. To estimate the rate of photolysis under UV (λ = 365 nm) and visible (λ ≥ 410 nm) light, the residual concentration of benzene was monitored by gas chromatography (GC). Both undoped/doped nanoparticles showed about 80 % of photolysis of benzene under UV light. However, under visible light irradiation Ag-doped TiO2 nanoparticles exhibited a photocatalytic reaction toward the photodegradation of benzene more efficient than that of bare TiO2. The enhanced photocatalytic reaction of Ag-doped TiO2 nanoparticles is attributed to the decrease in the activation energy and to the existence of Ag in the TiO2 host lattice, which increases the absorption capacity in the visible region by acting as an electron trapper and promotes charge separation of the photoinduced electrons (e−) and holes (h+). The use of Ag-doped TiO2 nanoparticles preserved the option of an environmentally benign photocatalytic reaction using visible light; These particles can be applicable to environmental cleaning applications.
고분자 전해질 막의 성능을 개선하고자 사용된 대표적인 무기물인 solid acid가 첨가된 복합막의 경우 고온에서 높은 열안정성을 나타내며 친수성이 강해지는 장점을 나타내지만 물에 녹는 단점을 가지고 있다. 그러므로 본 연구에서는 phosphotungstic acid(PWA)의 이온전도성을 증가시키며 물에 용해되는 성질을 제거하기 위하여 실리카 입자를 sol-gel법을 이용하여 술폰산기와 아민그룹을 도입시킨 입자를 제조한 후 sulfonated poly(arylene ether sulfone)(SPAES) 고분자에 첨가하여 복합막을 제조하였으며 특성평가가 이루어졌다.
The oxide films formed on etched aluminum foils play an important role as dielectric layers in aluminum electrolytic capacitors. Y2O3-doped ZrO2 (YZ) films were coated on the etched aluminum foils by sol-gel dip coating, and the electrical properties of YZ-coated Al foils were characterized. YZ films annealed at 450 oC were crystallized into a cubic phase, and as the Y2O3 doping content increased, the unit cell of ZrO2 expanded and the grain size decreased. The etch pits of Al foils were filled by YZ sol when it dried at atmospheric pressure after repeating for several times, but this step could essentially be avoided when being dried in a vacuum. YZ-coated foils indicated that the specific capacitance and dissipation factor were 2-2.5 μF/cm2 and 2-4 at 1 kHz, respectively, and the leakage current and withstanding voltage of films approximately 200 nm thick were 5 × 10−4A at 21 V and 22 V, respectively. After being anodized at 500 V, the foils exhibited a specific capacitance and dissipation factor of 0.6-0.7 μF/cm2 and 0.1-0.2, respectively, at 1 kHz, while the leakage current and withstanding voltage were 2 × 10−4 - 3 × 10−5 A at 400 V and 420-450 V, respectively. This suggests that YZ film is a promising dielectric that can be used in high voltage Al electrolytic capacitors.
PTMSP[Poly(1-trimethylsilyl-1-propyne)]에 TEOS (tetraethoxysilane), TMOS (tetramethoxysilane), MTMOS (methyltrimethoxysilane), 그리고 PTMOS (phenyltrimethoxysilane)의 함량을 0, 15, 20, 30 wt%로 달리하여 졸-겔법을 이용하 여 PTMSP-silica 복합막을 제조하였다. PTMSP-silica 복합막의 알콕시실란 함량에 따른 H2, N2의 기체투과도와 N2에 대한 H2의 이상 선택도를 조사하였다. H2와 N2의 투과도는 알콕시실란 함량이 0∼20 wt% 범위에서는 증가하다가 알콕시실란 함 량이 20∼30 wt% 범위에서는 감소하였다. N2에 대한 H2의 이상 선택도는 TEOS와 PTMOS의 함량이 0∼15 wt% 범위에서 는 감소하였으며, 15∼30 wt% 범위에서는 다시 증가하였다. Robeson upper bound와 비교할 때, PTMSP-silica 복합막은 TEOS 함량이 30 wt%, MTMOS 함량이 20 wt% 그리고 PTMOS 함량이 30 wt%에서 투과도와 이상 선택도가 동시에 향상된 것으로 나타났다.
The Mg-enriched magnesium aluminum silicate (MAS) glass is known for its higher mechanical strength and chemical resistance. Among such glasses, cordierite (Mg2Al4Si5O18) is well known to have a low thermal expansion and low melting point. Polycrystalline engineering ceramics such as alumina can be strengthened by a surface modification with low thermal expansion materials. The present study involves the synthesis of cordierite by a sol-gel process and investigates the effect of glass penetration on the surface of alumina. The cordierite powders were prepared from Al(OC3H7)3, Mg(OC2H5)2 and tetraethyl orthosilicate by hydrolysis and condensation reaction. The cordierite powders were characterized by X-ray diffraction (XRD, Rigaku), scanning electron microscope (SEM, JEOL: JSM-5610), energy dispersive spectroscopy (EDS, JEOL: JSM-5610), and universal testing machine (UTM, INSTRON). The X-ray diffraction patterns showed that the synthesized particles were μ-cordierite calcined at 1100˚C for 1 h. The shape of synthesized cordierite was changed from μ-cordierite to α-cordierite with increasing calcination temperature. Synthesized cordierite was used for surface modification of alumina. Cordierite powders penetrated deeply into the alumina sample along grain boundaries with increasing temperature. The results of surface modification tests showed that the strength of the prepared alumina sample increased after surface modification. The strength of a surface modified with synthesized cordierite increased the most, to about 134.6MPa.
Nanocomposites comprised of graphene oxide (GO) nanosheets and magnesium oxide (MgO) nanoparticles were synthesized by a sol-gel process. The synthesized samples were studied by X-ray powder diffraction, atomic force microscopy, transmission electron microscopy, and energy-dispersive X-ray analysis. The results show that the MgO nanoparticles, with an average diameter of 70 nm, are decorated uniformly on the surface of the GOs. By controlling the concentration of the MgO precursors and reaction cycles, it was possible to control the loading density and the size of the resulting MgO particles. Because the MgO particles are robustly anchored on the GO structure, the MgO/GOs nanocomposites will have future applications in the fields of adsorption and chemical sensing.
Nano-sized β-SiC nanoparticles were synthesized combined with a sol-gel process and a carbothermal process. TEOS and carbon black were used as starting materials for the silicon source and carbon source, respectively. SiO2 nanoparticles were synthesized using a sol-gel technique (Stober process) combined with hydrolysis and condensation. The size of the particles could be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of tetraethyl orthosilicate (TEOS) within the micro-emulsion. The average particle size and morphology of synthesized silicon dioxide was about 100nm and spherical, respectively. The average particles size and morphology of the used carbon black powders was about 20nm and spherical, respectively. The molar ratio of silicon dioxide and carbon black was fixed to 1:3 in the preparation of each combination. SiO2 and carbon black powders were mixed in ethanol and ball-milled for 12 h. After mixing, the slurries were dried at 80˚C in an oven. The dried powder mixtures were placed in alumina crucibles and synthesized in a tube furnace at 1400~1500˚C for 4 h with a heating rate of 10˚C/min under flowing Ar gas (160 cc/min) and furnace cooling down to room temperature. SiC nanoparticles were characterized by XRD, TEM, and SAED. The XRD results showed that high purity beta silicon carbide with excellent crystallinity was synthesized. TEM revealed that the powders are spherical shape nanoparticles with diameters ranging from 15 to 30 nm with a narrow distribution.
This paper describes the spherical ammonium diuranate gel particles which are the intermediated material of the microsphere for an VHTR(very high temperature reactor) nuclear fuel. The characteristics of the intermediate-ADU gel particles prepared by AWD(ageing, washing, and drying) and FB(fluidized-bed) apparatus were examined and compared in a sol-gel fabrication process. The electrical conductivity of washing filtrate from the FB treating and the surface area of dried-ADU gel particles were higher than those of AWD treating. Also, an internal pore volume in dried-ADU gel particles showed a more decrease in AWD treatment than FB treatment because of decomposition of PVA affected by the washing time. However, the internal microstructures of ADU gel particles were similar regardless of the process variation.
Fe doped TiO2 nanoparticles were prepared under high temperature and pressure conditions by mixture of metal nitrate solution and TiO2 sol. Fe doped TiO2 particles were reacted in the temperature range of 170 to 200˚C for 6 h. The microstructure and phase of the synthesized Fe doped TiO2 nanoparticles were studied by SEM (FE-SEM), TEM, and XRD. Thermal properties of the synthesized Fe doped TiO2 nanoparticles were studied by TG-DTA analysis. TEM and X-ray diffraction pattern shows that the synthesized Fe doped TiO2 nanoparticles were crystalline. The average size and distribution of the synthesized Fe doped TiO2 nanoparticles were about 10 nm and narrow, respectively. The average size of the synthesized Fe doped TiO2 nanoparticles increased as the reaction temperature increased. The overall reduction in weight of Fe doped TiO2 nanoparticles was about 16% up to ~700˚C; water of crystallization was dehydrated at 271˚C. The transition of Fe doped TiO2 nanoparticle phase from anatase to rutile occurred at almost 561˚C. The amount of rutile phase of the synthesized Fe doped TiO2 nanoparticles increased with decreasing Fe concentration. The effects of synthesis parameters, such as the concentration of the starting solution and the reaction temperature, are discussed.
Al2O3 has received wide attention with established use as a catalyst and growing application in structural or functional ceramic materials. On the other hand, the boehmite (AlO(OH)) obtained by sol-gel process has exhibited a decrease in surface area during phase transformation due to a decline in surface active site at high temperature. In this work, Al2O3-CuO/ZnO (ACZ) and Al2O3-CuO/CeO (ACC) composite materials were synthesized with aluminum isopropoxide, copper (II) nitrate hemi (pentahydrate), and cerium (III) nitrate hexahydrate or zinc (II) nitrate hexahydrate. Moreover, the Span 80 as the template block copolymer was added to the ACZ/ACC composition to make nano size particles and to keep increasing the surface area. The ACZ/ACC synthesized powders were characterized by Thermogravimetry-Differential Thermal analysis (TG/DTA), X-ray Diffractometer (XRD), Field-Emmision Scanning Electron Microscope (FE-SEM), Bruner-Emmett-Teller (BET) surface analysis and thermal electrical conductivity (ZEM-2:M8/L). An enhancement of surface area with the addition to Span 80 surfactant was observed in the ACZ powders from 105 m2/g to 142 m2/g, and the ACC powders from 103 m2/g to 140 m2/g, respectively.
Transparent conducting aluminum-doped ZnO thin films were deposited using a sol-gel process. In this study, the important deposition parameters were investigated thoroughly to determine the appropriate procedures to grow large area thin films with low resistivity and high transparency at low cost for device applications. The doping concentration of aluminum was adjusted in a range from 1 to 4 mol% by controlling the precursor concentration. The annealing temperatures for the pre-heat treatment and post-heat treatment was 250˚C and 400-600˚C, respectively. The SEM images show that Al doped and undoped ZnO films were quite uniform and compact. The XRD pattern shows that the Al doped ZnO film has poorer crystallinity than the undoped films. The crystal quality of Al doped ZnO films was improved with an increase of the annealing temperature to 600˚C. Although the structure of the aluminum doped ZnO films did not have a preferred orientation along the (002) plane, these films had high transmittance (> 87%) in the visible region. The absorption edge was observed at approximately 370 nm, and the absorption wavelength showed a blue-shift with increasing doping concentration. The ZnO films annealed at 500˚C showed the lowest resistivity at 1 mol% Al doping.
In this study, we investigated the unit process parameters in spherical kernel preparation. Nearly perfect spherical microspheres were obtained from the 0.6M of U-concentration in the broth solution, and the microstructure of the kernel appeared the good results in the calcining, reducing, and sintering processes. For good sphericity, high density, suitable microstructure, and no-crack final microspheres, the temperature control range in calcination process was , and the microstructure, the pore structure, and the density of kernel could be controlled in this temperature range. Also, the concentration changes of the ageing solution in aging step were not effective factor in the gelation of the liquid droplets, but the temperature change of the ageing solution was very sensitive for the final ADU gel particles
BaTiO3, powders were prepared by sol-gel process from different aging time and reaction temperature. Particle shape, size and crystal structure of prepared BaTiO3 powders were analyzed by SEM, XRD and FT-IR. Effect of aging time alternation didn't particularly show up. Spherical nano-sized BaTiO3 powders were obtained from condition more than reaction temperature 55℃, and obtained sintered BaTiO3 powders of tetragonal phase from heat-treatment at 1,100℃.
The transparent organic-inorganic hybrid films were prepared by the Sol-Gel process. PVP(polyvinylpyrrolidone) was used in organic component and TEOS(tetraethoxysilane) was used in inorganic component. HCI, CH3COOH, and NH4OH were used as the Sol-Gel catalyst. The characteristics according to not only the variation of organic and inorganic contents but also the variation of catalyst species and contents were investigated. On the whole, the compatibility was remained between organic and inorganic components, and also as the TEOS contents were increased, mostly the transparency and the mechanical, thermal properties were improved. In addition, as content of catalysts was increased, the films showed characteristics that were closer to PVP than silica. Although the transparency of films was preserved in HCI and CH3COOH, only the film containing more than 40wt% TEOS in NH4OH showed different phenomena.