(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.
Bismuth antimony telluride (BiSbTe) thermoelectric materials were successfully prepared by a spark plasma sintering process. Crystalline BiSbTe ingots were crushed into small pieces and then attrition milled into fine powders of about 300 nm ~ 2μm size under argon gas. Spark plasma sintering was applied on the BiSbTe powders at 240, 320, and 380˚C, respectively, under a pressure of 40 MPa in vacuum. The heating rate was 50˚C/min and the holding time at the sintering temperature was 10 min. At all sintering temperatures, high density bulk BiSbTe was successfully obtained. The XRD patterns verify that all samples were well matched with the Bi0.5Sb1.5Te3. Seebeck coefficient (S), electric conductivity (σ) and thermal conductivity (k) were evaluated in a temperature range of 25~300˚C. The thermoelectric properties of BiSbTe were evaluated by the thermoelectric figure of merit, ZT (ZT = S2σT/k). The grain size and electric conductivity of sintered BiSbTe increased as the sintering temperature increased but the thermal conductivity was similar at all sintering temperatures. Grain growth reduced the carrier concentration, because grain growth reduced the grain boundaries, which serve as acceptors. Meanwhile, the carrier mobility was greatly increased and the electric conductivity was also improved. Consequentially, the grains grew with increasing sintering temperature and the figure of merit was improved.
Hydroxyapatite (HA) is well known as a biocompatible and bioactive material. HA has been practically applied as bone graft materials in a range of medical and dental fields. In this study, two types of dense hydroxyapatite ceramics were prepared from natural bones and synthetic materials. The biocompatibility of HA ceramics for supporting osteoblast cell growth and cytotoxicity using an in vitro MG-63 cell line model were respectively evaluated. Artificial hydroxyapatite shows relative density of 93% with 1-2 μm after sintering, but a hydroxyapatite compact derived from bovine bone has low sintered density of 85% with a small content of MgO. Irrespective of the starting raw materials, both types of sintered hydroxyapatite displayed similar biocompatibility in the tests. FE-SEM observations showed that most MG-63 cells had a stellar shape and formed an intercellular matrix containing fibers on sintered HA. The cells were well attached and grown over the HA surface, indicating that there was no toxicity.
In order to improve osseointegration of dental implants with bone we studied an implant with holes inside its body to deliver bioactive materials based on a proposed patent. Bioactive materials can be selectively applied through holes to a patient according to diagnosis and the integration progress. After the bioactive material is applied, bone can grow into the holes to increase implant bonding and also enhance surface integration. In order to improve the concept and study the effect of bioactive material injection on implant integration, design optimization and integration research were undertaken utilizing the finite element method. A 2-dimensional simulation study showed that when bone grew into the holes after the bioactive material was injected, stress vertically distributed in the upper part of the implant was relieved and mild stress appeared at the opening of the injection holes. This confirmed the effect of the bioactive material and the contribution of the injection holes, but the maximum stress increased ten-fold at the opening. In order to reduce the maximum stress, the size, location, and the number of holes were varied and the effects were studied. When bioactive materials formed an interface layer between the implant and the mandible and four holes were filled with cortical and cancellous bones all the stress concentrated opposite to the loading side without holes disappeared. The stresses at the four outlets of the holes was mildly elevated but the maximum stress value was ten-fold greater compared to the case without the bioactive material.
Fe/SiO2 core-shell type composite nanoparticles have been synthesized using a reverse micelle process combined with metal alkoxide hydrolysis and condensation. Nano-sized SiO2 composite particles with a core-shell structure were prepared by arrested precipitation of Fe clusters in reverse micelles, followed by hydrolysis and condensation of organometallic precursors in micro-emulsion matrices. Microstructural and chemical analyses of Fe/SiO2 core-shell type composite nanoparticles were carried out by TEM and EDS. The size of the particles and the thickness of the coating could be controlled by manipulating the relative rates of the hydrolysis and condensation reaction of TEOS within the micro-emulsion. The water/surfactant molar ratio influenced the Fe particle distribution of the core-shell composite particles, and the distribution of Fe particles was broadened as R increased. The particle size of Fe increased linearly with increasing FeNO3 solution concentration. The average size of the cluster was found to depend on the micelle size, the nature of the solvent, and the concentration of the reagent. The average size of synthesized Fe/SiO2 core-shell type composite nanoparticles was in a range of 10-30 nm and Fe particles were 1.5-7 nm in size. The effects of synthesis parameters, such as the molar ratio of water to TEOS and the molar ratio of water to surfactant, are discussed.
This study evaluated the enhancement of microstructural and mechanical properties of a cross rolled Ni-10Cr alloy, comparing with conventionally rolled material. Cold rolling was carried out to 90% thickness reduction and the specimens were subsequently annealed at 700˚C for 30 min to obtain a fully recrystallized microstructure. Cross roll rolling was carried out at a tilted roll mill condition of 5˚ from the transverse direction in the RD-TD plane. In order to observe the deformed microstructures of the cold rolled materials, transmission electron microscopy was employed. For annealed materials after rolling, in order to investigate the grain boundary characteristic distributions, an electron back-scattering diffraction technique was applied. Application of cold rolling to the Ni-10Cr alloy contributed to notable grain refinement, and consequently the average grain size was refined from 135 μm in the initial material to 9.4 and 4.2 μm in conventionally rolled and cross rolled materials, respectively, thus showing more significantly refined grains in the cross rolled material. This refined grain size led to enhanced mechanical properties such as yield and tensile strengths, with slightly higher values in the cross rolled material. Furthermore, the<111>//ND texture in the CRR material was better developed compared to that of the CR material, which contributed to enhanced mechanical properties and formability.
Metal foam has many excellent properties, such as light weight, incombustibility, good thermal insulation, sound absorption, energy absorption, and environmental friendliness. It has two types of macrostructure, a closed-cell foam with sealed pores and an open-cell foam with open pores. The open-cell foam has a complex macrostructure consisting of an interconnected network. It can be exploited as a degradable biomaterial and a heat exchanger material. In this paper, open cell Mg alloy foams have been produced by infiltrating molten Mg alloy into porous pre-forms, where granules facilitate porous material. The granules have suitable strength and excellent thermal stability. They are also inexpensive and easily move out from open-cell foamed Mg-Al alloy materials. When the melt casting process used an inert gas, the molten magnesium igniting is resolved easily. The effects of the preheating temperature of the filler particle mould, negative pressure, and granule size on the fluidity of the open cell Mg alloy foam were investigated. With the increased infiltration pressure, preheat temperature and granule sizes during casting process, the molten AZ31 alloy was high fluidity. The optimum casting temperature, preheating temperature of the filler particle mould, and negative pressure were 750˚C, 400-500˚C, and 5000-6000 Pa, respectively, At these conditions the AZ31 alloy had good fluidity and castability with the longest infiltration length, fewer defects, and a uniform pore structure.
Co3O4, Al2O3 and Co3O4/Al2O3 mesoporous powders were prepared by a sol-gel method with starting matierals ofaluminum isopropoxide and cobalt (II) nitrate. A P123 template is employed as an active organic additive for improving thespecific surface area of the mixed oxide by forming surfactant micelles. A transition metal cobalt oxide supported on aluminawith and without P123 was tested to find the most active and selective conditions as a heterogeneous catalyst in the reactionof styrene epoxidation. A bBlock copolymer-P123 template was added to the staring materials to control physical and chemicalproperties. The properties of Co3O4/Al2O3 powder with and without P123 were characterized using an X-ray diffractometer(XRD), a Field-Emission Scanning Electron Microscope (FE-SEM), a Bruner-Emmertt-Teller (BET) surface analyzer, and 27AlMAS NMR spectroscopy. Powders with and without P123 were compared in catalytic tests. The catalytic activity and selectivitywere monitored by GC/MS, 1H, and 13C-NMR spectroscopy. The performance for the reaction of epoxidation of styrene wasobserved to be in the following order: [Co3O4/Al2O3 with P123-1173 K>Co3O4/Al2O3 with P123-973 K>Co3O4-973K>Co3O4/Al2O3-973 K>Co3O4/Al2O3 with P123-1473 K>Al2O3-973 K]. The existence of γ-alumina and the nature of thesurface morphology are related to catalytic activity.
The production of functional activated carbon materials starting from inexpensive natural precursors using environmentally friendly and economically effective processes has attracted much attention in the areas of material science and technology. In particular, the use of plant biomass to produce functional carbonaceous materials has attracted a great deal of attention in various aspects. In this study the preparation of activated carbon has been attempted from rice husks via a chemical activation-assisted microwave system. The rice husks were milled via attrition milling with aluminum balls, and then carbonized under purified N2. The operational parameters including the activation agents, chemical impregnation weight ratio of the calcined rice husk to KOH (1:1, 1:2 and 1:4), microwave power heating within irradiation time (3-5 min), and the second activation process on the adsorption capability were investigated. Experimental results were investigated using XRD, FT-IR, and SEM. It was found that the BET surface area of activated carbons irrespective of the activation agent resulted in surface area. The activated carbons prepared by microwave heating with an activation process have higher surface area and larger average pore size than those prepared by activation without microwave heating when the ratio with KOH solution was the same. The activation time using microwave heating and the chemical impregnation ratio with KOH solution were varied to determine the optimal method for obtaining high surface area activated carbon (1505 m2/g).