The theoretical capacity of silicon-based anode materials is more than 10 times higher than the capacity of graphite, so silicon can be used as an alternative to graphite anode materials. However, silicon has a much higher contraction and expansion rate due to lithiation of the anode material during the charge and discharge processes, compared to graphite anode materials, resulting in the pulverization of silicon particles during repeated charge and discharge. To compensate for the above issues, there is a growing interest in SiOx materials with a silica or carbon coating to minimize the expansion of the silicon. In this study, spherical silica (SiO2) was synthesized using TEOS as a starting material for the fabrication of such SiOx through heating in a reduction atmosphere. SiOx powder was produced by adding PVA as a carbon source and inducing the reduction of silica by the carbothermal reduction method. The ratio of TEOS to distilled water, the stirring time, and the amount of PVA added were adjusted to induce size and morphology, resulting in uniform nanosized spherical silica particles. For the reduction of the spherical monodisperse silica particles, a nitrogen gas atmosphere mixed with 5 % hydrogen was applied, and oxygen atoms in the silica were selectively removed by the carbothermal reduction method. The produced SiOx powder was characterized by FE-SEM to examine the morphology and size changes of the particles, and XPS and FT-IR were used to examine the x value (O/Si ratio) of the synthesized SiOx.
Silicon oxide (SiOx) has been considered one of the most promising anode materials for lithium-ion batteries due to having a higher capacity than the commercial graphite anodes. However, its practical application is hampered by very large volume variations. In this work, pyrolysis fuel oil is the carbon coating precursor, and physical vapor deposition (PVD) is performed on SiOx at 200 and 400 °C (SiOx@C 200 and SiOx@C 400), followed by carbonization at 950 °C. SiOx@C 200 has a carbon coating layer with a thickness of ~ 20 nm and an amorphous structure, while that of SiOx@C 400 is approximately 10 nm thick and has a more semigraphitic structure. The carbon-coated SiOx anodes display better charge–discharge performance than the pristine SiOx anode. In particular, SiOx@C 200 shows the highest reversible capacity compared with the other samples at high C-rates (2.0 and 5.0 C). Moreover, SiOx@C 200 exhibits excellent cycling stability with a capacity retention of 90.2% after 80 cycles at 1.0 C. This result is ascribed to the suppressed volume expansion by the PFO carbon coating on SiOx after PVD.
(3-mercaptopropyl)trimethoxysilane (MPTMS) was used as a silylation agent, and modified silica nanoparticles were prepared by solution polymerization. 2.0 g of silica nanoparticles, 150 ml of toluene, and 20 ml of MPTMS were put into a 300 ml flask, and these mixtures were dispersed with ultrasonic vibration for 60 min. 0.2 g of hydroquinone as an inhibitor and 1 to 2 drops of 2,6-dimethylpyridine as a catalyst were added into the mixture. The mixture was then stirred with a magnetic stirrer for 8 hrs. at room temperature. After the reaction, the mixture was centrifuged for 1 hr. at 6000rpm. After precipitation, 150 ml of ethanol was added, and ultrasonic vibration was applied for 30 min. After the ultrasonic vibration, centrifugation was carried out again for 1 hr. at 6000rpm. Organo-modification of silica nanoparticles with a γ-methacryloxypropyl functional group was successfully achieved by solution polymerization in the ethanol solution. The characteristics of the γ-mercaptopropyl modified silica nanoparticles (MPSN) were examined using X-ray photoelectron spectroscopy (XPS, THERMO VG SCIENTIFIC, MultiLab 2000), a laser scattering system (LSS, TOPCON Co., GLS-1000), Fourier transform infrared spectroscopy (FTIR, JASCO INTERNATIONL CO., FT/IR-4200), scanning electron microscopy (SEM, HITACHI, S-2400), an elemental analysis (EA, Elementar, Vario macro/micro) and a thermogravimetric analysis (TGA, Perkin Elmer, TGA 7, Pyris 1). From the analysis results, the content of the methacryloxypropyl group was 0.98 mmol/g and the conversion rate of acrylamide monomer was 93%. SEM analysis results showed that the organo-modification of ultra-fine particles effectively prevented their agglomeration and improved their dispensability.
We present the structural, optical, and electrical properties of amorphous silicon suboxide (a-SiOx) films grown on indium tin oxide glass substrates with a radio frequency magnetron technique from a polycrystalline silicon oxide target using ambient Ar. For different substrate-target distances (d = 8 cm and 10 cm), the deposition temperature effects were systematically studied. For d = 8cm, oxygen content in a-SiOx decreased with dissociation of oxygen onto the silicon oxide matrix; temperature increased due to enlargement of kinetic energy. For d = 10 cm, however, the oxygen content had a minimum between 150˚ and 200˚. Using simple optical measurements, we can predict a preferred orientation of liquid crystal molecules on a-SiOx thin film. At higher oxygen content (x > 1.6), liquid crystal molecules on an inorganic liquid crystal alignment layer of a-SiOx showed homogeneous alignment; however, in the lower case (x< 1.6), liquid crystals showed homeotropic alignment.
일반적으로 TFT(thin film transistor)의 유전체막으로 실리콘 질화막(Si3N4)이나 실리콘 산화막(SiO2)을 200-300˚C의 온도에서 증착을 하게 되는데 본 연구에서는 비정질 실리콘과 유전체막 사이의 계면 특성 특히 계면의 거칠기를 향상시키기 위해서 기존의 증착법이 아니라 비정질 실리콘(a-Si:H)과 산소 ECR 플라즈마의 반응에 의한 산화 막의 성장법을 시도했는데, 이때 기판은 의도적으로 가열하지 않았으며 특히 본 연구에서는 기존의 시도와는 달리 ECR 플라즈마를 형성할 때 마이크로파 전력에 pulse를 가하는 방법을 최초로 시도했고, 계면에 불순물의 혼입을 최대한으로 줄이기 위해서 진공을 파괴하지 않은 상태로 산화막을 연속적으로 성장시키는 방법을 이용했다. Pulse를 가했을 경우에는 pulse를 가하지 않은 경우에 비해서 화학양론적 측면, 유전상수, 산화막의 표면 평탄도 등에서 우수한 산화막이 성장했으며, 특히 비정질 실리콘과 유전체막 사이의 계면 특성을 반영하는 산화막의 표면 평탄도가 1/3정도로 획기적으로 줄어들었다.