Olivine is a complete solid solution of fayalite and forsterite that is abundant in Earth and extraterrestrial materials such as rocky planets, meteorites, asteroids, and interplanetary dust. Due to the wide range of olivine compositions, diverse olivine standards are required for quantitative mineralogical analysis of olivine-bearing materials. Olivine standards were synthesized using an electric furnace and stainless steel tubes at temperatures ranging from 1000~1100 ℃. Overall, olivine was synthesized covering the full range of composition, with some synthetic impurities and unreacted material. The synthesized olivine showed a linear increase in the unit cell dimension in proportion to the molar ratio of fayalite in the starting materials, and the diffraction intensity was consistent with that of natural olivine. However, iron-rich synthetic olivine samples tend to have a higher content of impurity, suggesting that not all synthetic olivine can be used as a standard material yet, and improvements in the synthesis process, such as using high purity starting materials and control of reaction time and temperature, are required.
Proceedings of the Korean Vacuum Society Conference
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2012.08a
/
pp.386-386
/
2012
For white light emitting diode (LED) applications, it has been reported that Y3Al5O12:Ce3+ (YAG:Ce) in nano-sized phosphor performs better than it does in micro-sized particles. This is because nano-sized YAG:Ce can reduce internal light scattering when coated onto a blue LED surface. Recently, there have been many reports on the synthesis of nano-sized YAG particles using bottom-up method, such as co-precipitation method, sol-gel process, hydrothermal method, solvothermal method, and glycothermal method. However, there has been no report using top-down method. Top-down method has advantages than bottom-up method, such as large scale production and easy control of doping concentration and particle size. Therefore, in this study, nano-sized YAG:Ce phosphors were synthesized by a high energy beads milling process with varying beads size, milling time and milling steps. The beads milling process was performed by Laboratory Mill MINICER with ZrO2 beads. The phase identity and morphology of nano-sized YAG:Ce were characterized by X-ray powder diffraction (XRD) and field-emission scanning electron microscopy (FESEM), respectively. By controlling beads size, milling time and milling steps, we synthesized a size-tunable and uniform nano-sized YAG:Ce phosphors which average diameters were 100, 85 and 40 nm, respectively. After milling, there was no impurity and all of the peaks were in good agreement with YAG (JCPDS No. 33-0040). Luminescence and quantum efficiency (QE) of nano-sized YAG:Ce phosphors were measured by fluorescence spectrometer and QE measuring instrument, respectively. The synthesized YAG:Ce absorbed light efficiently in the visible region of 400-500 nm, and showed single broadband emission peaked at 550 nm with 50% of QE. As a result, by considering above results, high energy beads milling process could be a facile and reproducible synthesis method for nano-sized YAG:Ce phosphors.
This paper presents an investigation of the mechanical and microstructural properties of Class F fly ash based geopolymer containing sodium sulfate as an additive. Sodium sulfate was used as an chemical additive at the dosage levels of 0, 2, 4, and 6wt% of fly ash. Sodium hydroxide and sodium silicate solutions were used to activate fly ash. The compressive strengths of geopolymer pastes were measured at the age of 28 days. The microstructures of the geopolymer pastes were examined using XRD, MIP and SEM tests. The additions of 2wt% and 4wt% sodium sulfate produced geopolymers with high strength, while increasing the dosage of levels to 6% resulted in almost no changes in strength, comparing with the control geopolymer. The optimum increase in strength was obtained with the addition of 4wt% sodium sulfate. As the amount of sodium sulfate is increased, no additional crystalline phase was detected and no change of amorphous phase indicated despite the change in the strength development. The increase in the strength was due to the change of pore size distribution in samples. As addition of sodium sulfate altered the morphologies of reactive productions and Si/Al ratios of the reaction products, the strengths were thus affected. It was found that the strengths of geopolymer were larger for lower Si/Al ratios of reaction products formed in samples. The optimal amount of sodium sulfate in the fly ash based geopolymer helps to improve mechanical properties of the geopolymer, on the other hand, the high percentage of sodium sulfate could exist as an impurity in the geopolymer and hinder the geopolymer reaction.
Kim, Jung Hyun;Kim, Min Young;Kwon, Eun Kyung;Lee, Kwang Moon;Choi, Don Woong
YAKHAK HOEJI
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v.59
no.3
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pp.98-106
/
2015
Analytical method for related substances can be categorized into two methods depending on the necessity of reference standard (RS). The analytical method of related substances with RS is fast and accurate, but it's very expensive and technically difficult to synthesize RS due to their complicated structure. Another method is using relative retention time (RRT) and relative response factor (RRF) which are already validated with RS. Validation of this method is not easy and time consuming, but once it has been developed, it can save cost and time. In this study, we developed the analytical method for related substances of fenofibrate using RRT and RRF. We validated the method by evaluating specificity, linearity, accuracy and precision according to the "Manual for Guideline Application for Validation of Analytical Procedures" of MFDS. Also, we calculated RRT and RRF between fenofibrate and fenofibrate related substances. The results of this study showed high specificity for fenofibrate and fenofibrate related substances. Correlation coefficient(r) of all substances were more than 0.99, and the recovery of fenofibrate, fenofibrate related substance I, II and III were 99.44%, 100.84%, 99.14% and 101.58%, respectively. Precision of fenofibrate and its related substances were ranged between RSD 0.29% and 0.93%. Quantification limits of fenofibrate, fenofibrate related substance I, II and III were determined to be $0.03{\mu}g/ml$, $0.05{\mu}g/ml$, $0.04{\mu}g/ml$ and $0.02{\mu}g/ml$, respectively by confirming signal to noise ratio of each chromatogram. The RRT for fenofibrate related substance I, II and III were determined to be 0.35, 0.41 and 1.34, respectively. Also, the RRF for fenofibrate related substance I, II and III were determined to be 1.28, 0.98 and 0.79, respectively. The developed method was applied to determine contents for fenofibrate related substances in commercial fenofibrate (active pharmaceutical ingredient). As a result, developed analytical methods of related substances will be used for revising the monograph of fenofibrate in Korean Pharmacopoeia revision and contribute quality control of drugs by improving cost and time consuming problem of RS.
Kim, Young-Soon;Shin, Jiho;Kim, Hyung-Il;Cho, Joong-Hee;Seo, Hyung-Ki;Kim, Gil-Sung;Shin, Hyung-Shik
Korean Chemical Engineering Research
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v.43
no.4
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pp.495-502
/
2005
Copper was plated on the tungsten substrate by use of a direct copper electroless plating. The optimum deposition conditions were found to be with a concentration of $CuSO_4$ 7.615 g/L, EDTA of 10.258 g/L, and glyoxylic acid of 7 g/L, respectively. The solution temperature was maintained at $60^{\circ}C$. The pH was varied from 11.0 to 12.8. After the deposition, the properties of the copper film were investigated with X-ray diffractometer (XRD), Field emission secondary electron microscope (FESEM), Atomic force microscope (AFM), X-ray photoelectron spectroscope (XPS), and Rutherford backscattering spectroscope (RBS). The best deposition condition was founded to be the solution pH of 11.8. In the case of 10 min deposition at the pH of 11.8, the grain shape was spherical, Cu phase was pure without impurity peak ($Cu_2O$ peak), and the surface root mean square roughness was about 11 nm. The thickness of the film turned out to be 140 nm after deposition for 12 min and the deposition rate was found to be about 12 nm/min. Increase in pH induced a formation of $Cu_2O$ phase with a long rectangular grain shape. The pH control seems to play an important role for the orientation of Cu in electroless deposition. The deposited copper concentration was 99 atomic percent according to RBS. The resulting Cu/W film yielded a good adhesive strength, because Cu/W alloy forms during electroless deposition.
Kim, Dong-Pyo;Woo, Jong-Chang;Um, Doo-Seng;Yang, Xue;Kim, Chang-Il
Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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2008.11a
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pp.363-363
/
2008
The development of dry etching process for sapphire wafer with plasma has been key issues for the opto-electric devices. The challenges are increasing control and obtaining low plasma induced-damage because an unwanted scattering of radiation is caused by the spatial disorder of pattern and variation of surface roughness. The plasma-induced damages during plasma etching process can be classified as impurity contamination of residual etch products or bonding disruption in lattice due to charged particle bombardment. Therefor, fine pattern technology with low damaged etching process and high etch rate are urgently needed. Until now, there are a lot of reports on the etching of sapphire wafer with using $Cl_2$/Ar, $BCl_3$/Ar, HBr/Ar and so on [1]. However, the etch behavior of sapphire wafer have investigated with variation of only one parameter while other parameters are fixed. In this study, we investigated the effect of pressure and other parameters on the etch rate and the selectivity. We selected $BCl_3$ as an etch ant because $BCl_3$ plasmas are widely used in etching process of oxide materials. In plasma, the $BCl_3$ molecule can be dissociated into B radical, $B^+$ ion, Cl radical and $Cl^+$ ion. However, the $BCl_3$ molecule can be dissociated into B radical or $B^+$ ion easier than Cl radical or $Cl^+$ ion. First, we evaluated the etch behaviors of sapphire wafer in $BCl_3$/additive gases (Ar, $N_2,Cl_2$) gases. The behavior of etch rate of sapphire substrate was monitored as a function of additive gas ratio to $BCl_3$ based plasma, total flow rate, r.f. power, d.c. bias under different pressures of 5 mTorr, 10 mTorr, 20 mTorr and 30 mTorr. The etch rates of sapphire wafer, $SiO_2$ and PR were measured with using alpha step surface profiler. In order to understand the changes of radicals, volume density of Cl, B radical and BCl molecule were investigated with optical emission spectroscopy (OES). The chemical states of $Al_2O_3$ thin films were studied with energy dispersive X-ray (EDX) and depth profile anlysis of auger electron spectroscopy (AES). The enhancement of sapphire substrate can be explained by the reactive ion etching mechanism with the competition of the formation of volatile $AlCl_3$, $Al_2Cl_6$ or $BOCl_3$ and the sputter effect by energetic ions.
Kim, Myung-Chan;Heo, Cheol-Ho;Boo, Jin-Hyo;Cho,Yong-Ki;Han, Jeon-Geon
Proceedings of the Korean Vacuum Society Conference
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1999.07a
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pp.211-211
/
1999
Titanium nitride (TiN) thin films have useful properties including high hardness, good electrical conductivity, high melting point, and chemical inertness. The applications have included wear-resistant hard coatings on machine tools and bearings, decorative coating making use of the golden color, thermal control coatings for widows, and erosion resistant coatings for spacecraft plasma probes. For all these applications as feature sizes shrink and aspect ratios grow, the issue of good step coverage becomes increasingly important. It is therefore essential to manufacture conformal coatings of TiN. The growth of TiN thin films by chemical vapor deposition (CVD) is of great interest for achieving conformal deposition. The most widely used precursor for TiN is TiCl4 and NH3. However, chlorine impurity in the as-grown films and relatively high deposition temperature (>$600^{\circ}C$) are considered major drawbacks from actual device fabrication. To overcome these problems, recently, MOCVD processes including plasma assisted have been suggested. In this study, therefore, we have doposited Ti(C, N) thin films on Si(100) and D2 steel substrates in the temperature range of 150-30$0^{\circ}C$ using tetrakis diethylamido titanium (TDEAT) and titanium isopropoxide (TIP) by pulsed DC plamsa enhanced metal-organic chemical vapor deposition (PEMOCVD) method. Polycrystalline Ti(C, N) thin films were successfully grown on either D2 steel or Si(100) surfaces at temperature as low as 15$0^{\circ}C$. Compositions of the as-grown films were determined with XPS and RBS. From XPS analysis, thin films of Ti(C, N) with low oxygen concentration were obtained. RBS data were also confirmed the changes of stoichiometry and microhardness of our films. Radical formation and ionization behaviors in plasma are analyzed by optical emission spectroscopy (OES) at various pulsed bias and gases conditions. H2 and He+H2 gases are used as carrier gases to compare plasma parameter and the effect of N2 and NH3 gases as reactive gas is also evaluated in reduction of C content of the films. In this study, we fond that He and H2 mixture gas is very effective in enhancing ionization of radicals, especially N resulting is high hardness. The higher hardness of film is obtained to be ca. 1700 HK 0.01 but it depends on gas species and bias voltage. The proper process is evident for H and N2 gas atmosphere and bias voltage of 600V. However, NH3 gas highly reduces formation of CN radical, thereby decreasing C content of Ti(C, N) thin films in a great deal. Compared to PVD TiN films, the Ti(C, N) film grown by PEMOCVD has very good conformability; the step coverage exceeds 85% with an aspect ratio of more than 3.
Kim, Gyeong-Jung;Hong, Seung-Hwi;Kim, Yong-Seong;Lee, U;Kim, Yeong-Heon;Seo, Se-Yeong;Jang, Jong-Sik;Sin, Dong-Hui;Choe, Seok-Ho
Proceedings of the Korean Vacuum Society Conference
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2010.08a
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pp.297-297
/
2010
Precise control of the position and density of doping elements at the nanoscale is becoming a central issue for realizing state-of-the-art silicon-based optoelectronic devices. As dimensions are scaled down to take benefits from the quantum confinement effect, however, the presence of interfaces and the nature of materials adjacent to silicon turn out to be important and govern the physical properties. Utilization of visible light is a promising method to overcome the efficiency limit of the crystalline Si solar cells. Si quantum dots (QDs) have been proposed as an emission source of visible light, which is based on the quantum confinement effect. Light emission in the visible wavelength has been reported by controlling the size and density of Si QDs embedded within various types of insulating matrix. For the realization of all-Si QD solar cells with homojunctions, it is prerequisite not only to optimize the impurity doping for both p- and n-type Si QDs, but also to construct p-n homojunctions between them. In this study, XPS and SIMS were used for the development of p-type and n-type Si quantum dot solar cells. The stoichiometry of SiOx layers were controlled by in-situ XPS analysis and the concentration of B and P by SIMS for the activated doping in Si nano structures. Especially, it has been experimentally evidenced that boron atoms in silicon nanostructures confined in SiO2 matrix can segregate into the Si/$SiO_2$ interfaces and the Si bulk forming a distinct bimodal spatial distribution. By performing quantitative analysis and theoretical modelling, it has been found that boron incorporated into the four-fold Si crystal lattice can have electrical activity. Based on these findings, p-type Si quantum dot solar cell with the energy-conversion efficiency of 10.2% was realized from a [B-doped $SiO_{1.2}$(2 nm)/$SiO_2(2\;nm)]^{25}$ superlattice film with a B doping level of $4.0{\times}10^{20}\;atoms/cm^2$.
Journal of the Korea Academia-Industrial cooperation Society
/
v.21
no.4
/
pp.596-601
/
2020
Silicon carbide is considered a potentially useful material for high-temperature electronic devices because of its large band gap energy and p-type or n-type conduction that can be controlled by impurity doping. Accordingly, the thermoelectric properties of -SiC powder prepared by refined diatomite were investigated for high value-added applications of natural diatomite. -SiC powder was synthesized by a carbothermal reduction of the SiO2 in refined diatomite using carbon black. An acid-treatment process was then performed to eliminate the remaining impurities (Fe, Ca, etc.). n-Type semiconductors were fabricated by sintering the pressed powder at 2000℃ for 1~5h in an N2 atmosphere. The electrical conductivity increased with increasing sintering time, which might be due to an increase in carrier concentration and improvement in grain-to-grain connectivity. The carrier compensation effect caused by the remaining acceptor impurities (Al, etc.) in the obtained -SiC had a deleterious influence on the electrical conductivity. The absolute value of the Seebeck coefficient increased with increasing sintering time, which might be due to a decrease in the stacking fault density accompanied by grain or crystallite growth. On the other hand, the power factor, which reflects the thermoelectric conversion efficiency of the present work, was slightly lower than that of the porous SiC semiconductors fabricated by conventional high-purity -SiC powder, it can be stated that the thermoelectric properties could be improved further by precise control of an acid-treatment process.
One of today's very critical and sensitive accurate accelerometer which can be used higher temperature than $200^{\circ}C$ and corrosive environment, is particularly demanded for automotive engine. Because silicon is a material of large temperature dependent coefficient, and the piezoresistors are isolated with p-n junctions, and its leakage current increase with temperature, the performance of the silicon accelerometer degrades especially after $150^{\circ}C$. In this paper, The temperature characteristic of a accelerometer using silicon on insulator (SOI) structure is studied theoretically, and compared with experimental results. The temperature coefficients of sensitivity and offset voltage (TCS and TCO) are related to some factors such as thermal residual stress, and are expressed numerically. Thermal stress analysis of the accelerometer has also been carried out with the finite-element method(FEM) simulation program ANSYS. TCS of this accelerometer can be reduced to control the impurity concentration of piezoresistors, and TCO is related to factors such as process variation and thermal residual stress on the piezoresistors. In real packaging, The avarage thermal residual stress in the center support structure was estimated at around $3.7{\times}10^4Nm^{-2}^{\circ}C^{-1}$ at sensing resistor. The simulated ${\gamma}_{pT}$ of the center support structure was smaller than one-tenth as compared with that of the surrounding support structure.
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