• Advances in nano research
• /
• v.1 no.3
• /
• pp.159-169
• /
• 2013

A preparation method for gadolinium compound (GdC) nanoparticles coated with silica ($GdC/SiO_2$) is proposed. GdC nanoparticles were prepared with a homogeneous precipitation method at $80^{\circ}C$ using $1.0{\times}10^{-3}$ M $Gd(NO_3)_3$, 0.5 M urea and $0-3.0{\times}10^{-4}$ M ethylenediarinnetetraacetic acid disodium salt dihydrate (ETDA) in water. As a result of preparation at various EDTA concentrations, GdC nanoparticles with a size as small as $40.5{\pm}6.2$ nm, which were colloidally stable, were prepared at an EDTA concentration of $2.0{\times}10^{-4}$ M. Silica-coating of the GdC nanoparticles was performed by a St$\ddot{o}$ber method at $35^{\circ}C$ using $1.0-10.0{\times}10^{-3}$ M tetraethylorthosilicate (TEOS), 11 M $H_2O$ and $1.5{\times}10^{-3}$ M NaOH in ethanol in the presence of $1.0{\times}10^{-3}$ M GdC nanoparticles. Performance of preparation at various TEOS concentrations resulted in production of $GdC/SiO_2$ particles with an average size of $106.1{\pm}11.2$ nm at a TEOS concentration of $5.0{\times}10^{-3}$ M. The gadolinium (Gd) concentration of $1.0{\times}10^{-3}$ M in the as-prepared $GdC/SiO_2$ particle colloid solution was increased up to a Gd concentration of 0.2 M by concentrating with centrifugation. The core-shell structure of $GdC/SiO_2$ particles was undamaged, and the colloid solution was still colloidally stable, even after the concentrating process. The concentrated $GdC/SiO_2$ colloid solution showed images of X-ray and magnetic resonance with contrast as high as commercial Gd complex contrast agents.

• Applied Chemistry for Engineering
• /
• v.26 no.3
• /
• pp.362-365
• /
• 2015

Silica encapsulated ZnSe quantum dots (QDs) were prepared by employing two microemulsion systems: AOT/water/cyclohexane microemulsions containing ZnSe quantum dots with NP5/water/cyclohexane microemulsions containing tetraethylorthosilicate (TEOS). Using this method, cubic zinc blende nanoparticles (3 nm in diameter) were synthesized and encapsulated by silica nanoparticles (20 nm in diameter). The temperature dependence of photoluminescence (PL) for silica-encapsulated ZnSe QDs was investigated to evaluate this material as a temperature sensor media. The fluorescence emission intensity of silica-encapsulated ZnSe nanoparticles (NPs) was decreased with an increase of ambient temperature over the range from $30^{\circ}C$ to $60^{\circ}C$ and a linear relationship between the temperature and the emission intensity was observed. In addition, the temperature dependence of PL intensity for silica-encapsulated ZnSe NPs showed a reversible pattern on ambient temperature. A reversible temperature dependence of the luminescence combined with its insensitivity toward quenching by oxygen due to silica coating established this material as an attractive media for temperature sensor applications.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 2011.10a
• /
• pp.23-23
• /
• 2011

Chemical-Mechanical Planarization (CMP) 공정이란 화학적 반응 및 기계적인 힘이 복합적으로 작용하여 표면을 평탄화하는 공정이다. 이러한 CMP 공정은 반도체 산업에서 회로의 고집적화와 다층구조를 형성하기 위하여 도입되었으며 반도체 제조를 위한 필수공정으로 그 중요성이 강조되고 있다. 특히 최근에는 Inter-Level Dielectric (ILD)의 형성과 Shallow Trench Isolation (STI) 공정에서실리콘 산화막을 평탄화하기 위한 CMP 공정에 대해 연구가 활발히 이루어지고 있다. 그러나 CMP 공정 후 scratch, pitting corrosion, contamination 등의 Defect가 발생하는 문제점이 존재한다. 이 중에서도 scratch는 기계적, 열적 스트레스에 의해 생성된 패드의 잔해, 슬러리의 잔유물, 응집된 입자 등에 의해 표면에 형성된다. 반도체 공정에서는 다양한 종류의 실리콘 산화막이 사용되고 gks이러한 실리콘 산화막들은 종류에 따라 경도가 다르다. 따라서 실리콘 산화막의 경도에 따른 CMP 공정 및 이로 인한 Scratch 발생에 관한 연구가 필요하다고 할 수 있다. 본 연구에서는 scratch 형성의 거동을 알아보기 위하여 boronphoshposilicate glass (BPSG), plasma enhanced chemical vapor deposition (PECVD) tetraethylorthosilicate (TEOS), high density plasma (HDP) oxide의 3가지 실리콘 산화막의 기계적 성질 및 이에 따른 CMP 공정에 대한 평가를 실시하였다. CMP 공정 후 효율적인 scratch 평가를 위해 브러시를 이용하여 1차 세정을 실시하였으며 습식세정방법(SC-1, DHF)으로 마무리 하였다. Scratch 개수는 Particle counter (Surfscan6200, KLA Tencor, USA)로 측정하였고, 광학현미경을 이용하여 형태를 관찰하였다. Scratch 평가를 위한 CMP 공정은 실험에 사용된 3가지 종류의 실리콘 산화막들의 경도가 서로 다르기 때문에 동등한 실험조건 설정을 위해 동일한 연마량이 관찰되는 조건에서 실시하였다. 실험결과 scratch 종류는 그 형태에 따라 chatter/line/rolling type의 3가지로 분류되었다 BPSG가 다른 종류의 실리콘 산화막에 비해 많은 수에 scratch가 관찰되었으며 line type이 많은 비율을 차지한다는 것을 확인하였다. 또한 CMP 공정에서 압력이 증가함에 따라 chatter type scratch의 길이는 짧아지고 폭이 넓어지는 것을 확인하였다. 본 연구를 통해 실리콘 산화막의 경도에 따른 scratch 형성 원리를 파악하였다.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 2003.11a
• /
• pp.136-136
• /
• 2003

In fiber optic networks, system size and cost can be significantly reduced by development of optical components through planar optical waveguides. One important step to realize the compact optical devices is to develop planar optical amplifier to compensate the losses in splitter or other components. Planar amplifier provides optical gain in devices less than tens of centimeters long, as opposed to fiber amplifiers with lengths of typically tens of meters. To achieve the same amount of gain between the planar and fiber optical amplifier, much higher Er doping levels responsible for the gain than in the fiber amplifier are required due to the reduced path length. These doping must be done without the loss of homogeniety to minimize Er ion-ion interactions which reduce gain by co-operative upconversion. Sol-gel process has become a feasible method to allow the incorporation of Er ion concentrations higher than conventional glass melting methods. In this work, Er-doped $SiO_2$-A1$_2$ $O_3$ films were prepared by two different method via sol -Eel process. Tetraethylorthosilicate(TEOS)/aluminum secondary butoxide [Al (OC$_4$ $H_{9}$)$_3$], methacryloxypropylcnethoxysaane(MPTS)/aluminum secondary butofde [Al(OC$_4$ $H_{9}$)$_3$] systems were used as starting materials for hosting Er ions. Er-doped $SiO_2$-A1$_2$ $O_3$ films obtahed after heat-treating, coatings on Si substrate were characterized by X-ray din action, FT-IR, and N-IR fluorescence spectroscopy. The luminescence properties for two different processing procedure will be compared and discussed from peak intensity and life time.

• Proceedings of the Materials Research Society of Korea Conference
• /
• 2011.05a
• /
• pp.34.2-34.2
• /
• 2011

The demand for Ru has been increasing in the electronic, chemical and semiconductor industry. Chemical mechanical planarization (CMP) is one of the fabrication processes for electrode formation and barrier layer removal. The abrasive particles can be easily contaminated on the top surface during the CMP process. This can induce adverse effects on subsequent patterning and film deposition processes. In this study, a post Ru CMP cleaning solution was formulated by using sodium periodate as an etchant and citric acid to modify the zeta potential of alumina particles and Ru surfaces. Ru film (150 nm thickness) was deposited on tetraethylorthosilicate (TEOS) films by the atomic layer deposition method. Ru wafers were cut into $2.0{\times}2.0$ cm pieces for the surface analysis and used for estimating PRE. A laser zeta potential analyzer (LEZA-600, Otsuka Electronics Co., Japan) was used to obtain the zeta potentials of alumina particles and the Ru surface. A contact angle analyzer (Phoenix 300, SEO, Korea) was used to measure the contact angle of the Ru surface. The adhesion force between an alumina particle and Ru wafer surface was measured by an atomic force microscope (AFM, XE-100, Park Systems, Korea). In a solution with citric acid, the zeta potential of the alumina surface was changed to a negative value due to the adsorption of negative citrate ions. However, the hydrous Ru oxide, which has positive surface charge, could be formed on Ru surface in citric acid solution at pH 6 and 8. At pH 6 and 8, relatively low particle removal efficiency was observed in citric acid solution due to the attractive force between the Ru surface and particles. At pH 10, the lowest adhesion force and highest cleaning efficiency were measured due to the repulsive force between the contaminated alumina particle and the Ru surface. The highest PRE was achieved in citric acid solution with NaIO4 below 0.01 M at pH 10.

• Journal of the Korean Ceramic Society
• /
• v.54 no.1
• /
• pp.49-54
• /
• 2017

In this study, based on hydrolysis and condensation via $St{\ddot{o}}ber$ process of sol-gel method, synthesis of mono-dispersed silica nanoparticles was carried out with hydrophilic solvent. This operation was expected to be a more simplified process than that with organic solvent. Based on the sol-gel method, which involves simply controlling the particle size, the particle size of the synthesized silica specimens were ranged from 30 to 300 nm by controlling the composition of tetraethylorthosilicate (TEOS), DI water and ammonia solution, and by varying the stirring speeds while maintaining a fixed amount of ethanol. Increasing the content of DI water and decreasing the content of ammonia caused the particle size to decrease, while controlling the stirring speed at a high level of RPMs enabled a decrease of the particle size. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) were utilized to investigate the success factors for synthesizing process; Field emission scanning electron microscopy (FE-SEM) was used to study the effects of the size and morphology of the synthesized particles. To analyze the dispersion properties, zeta potential and particle size distribution (PSD) analyses were utilized.

• Korean Chemical Engineering Research
• /
• v.47 no.3
• /
• pp.275-280
• /
• 2009

The direct incorporation of vanadium into the three-dimensional(3-D) cubic Ia3d mesostructure designated as V-KIT-6 was carried out hydrothermally using a Pluronic P123 and n-butanol as the structure-directing mixture, tetraethylorthosilicate(TEOS) as the silica source and $NH_4VO_3$ as the vanadium source. The obtained V-KIT-6 showed a very high specific surface area ${\sim}1,000m^2/g$ with tunable pore diameters in narrow distribution of sizes ~6.0 nm. The coordination and nature of V sites in V-KIT-6 are characterized by $^{51}V$-spin-echo NMR analysis. The calcined V-KIT-6 materials showed excellent catalytic activity in the direct oxidation of styrene using tert-butyl hydroperoxide(TBHP) as an oxidant.

• Korean Chemical Engineering Research
• /
• v.45 no.6
• /
• pp.611-618
• /
• 2007

We demonstrate the sol-gel coating technique of colloidal clusters for producing hollow micro-particles with complex morphologies. Cross-linked amidine polystyrene (PS) microspheres were synthesized by emulsifier-free emulsion copolymerization of styrene and divinylbenzene. The amidine PS particles were self-organized inside toluene-in-water emulsion droplets to produce large quantities of colloidally stable clusters. These clusters were coated with thin silica shell by sol-gel reaction of tetraethylorthosilicate (TEOS) and ammonia, and the organic polystyrene cores were removed by calcination at high temperature to generate nonspherical hollow micro-particles with complex morphologies. This process can be used to prepare hollow particles with shapes such as doublets, tetrahedra, icosahedra, and others.

• Membrane Journal
• /
• v.25 no.2
• /
• pp.115-122
• /
• 2015

$SiO_2{\cdot}B_2O_3$ was prepared by trimethylborate (TMB)/tetraethylorthosilicate (TEOS) mole ratio 0.01 at $800^{\circ}C$. PDMS[poly(dimethysiloxane)]-$SiO_2{\cdot}B_2O_3$ composite membranes were prepared by adding porous $SiO_2{\cdot}B_2O_3$ to PDMS. To investigate the characteristics of PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane, we observed PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane using TG-DTA, FT-IR, BET, X-ray, and SEM. PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was studied on the permeabilities of $H_2$ and $N_2$ and the selectivity ($H_2/N_2$). Following the results of TG-DTA, BET, X-ray, FT-IR, $SiO_2{\cdot}B_2O_3$ was the amorphous porous $SiO_2{\cdot}B_2O_3$ with $247.6868m^2/g$ surface area and $37.7821{\AA}$ the mean of pore diameter. According to the TGA measurements, the thermal stability of PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was enhanced by inserting $SiO_2{\cdot}B_2O_3$. SEM observation showed that the size of dispersed $SiO_2{\cdot}B_2O_3$ in the PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was about $1{\mu}m$. The increasing of $SiO_2{\cdot}B_2O_3$ content in PDMS leaded the following results in the gas permeation experiment: the permeability of both $H_2$ and $N_2$ was increased, and the permeability of $H_2$ was higher than $N_2$, but the selectivity($H_2/N_2$) was decreased.

• Applied Chemistry for Engineering
• /
• v.10 no.8
• /
• pp.1180-1185
• /
• 1999

Modispersed silica fine particles were produced from the hydrolysis of $Si(OC_2H_5)_4$ by using batch-semibatch mixed systems. Four types of mixed process, i.e., batch-batch, batch-semibatch, semibatch-batch, semibatch-semibatch, were used in order to measure mean particle size, particle size distribution, yield, and packing density. As a result of the test, silica particles prepared by semibatch-semibatch process were larger than those prodeced from any other systems in particle size and yield. On the other hand, silica particles prepared by batch-semibatch process were better than those produced from any other systems in particle size distribution and packing density. Especially, it was found that particle size of $SiO_2$ prepared by semibatch-batch process decreased with increasing the reaction time. Therefore, batch-semibatch process was a successful method for controlling the size, i.e., a narrow distribution of a particle size which ranges to several microns.