• Applied Chemistry for Engineering
• /
• v.25 no.5
• /
• pp.455-462
• /
• 2014

This work investigated the hydrophobic coating of silicate yellow phosphor powder in the form of divalent europium-activated strontium orthosilicate ($Sr_2SiO_4:Eu^{2+}$) by using an atmospheric pressure dielectric barrier discharge (DBD) plasma with argon as a carrier and hexamethyldisiloxane (HMDSO), toluene and n-hexane as precursors. After the plasma treatment of the phosphor powder, the lattice structure of orthosilicate was not altered, as confirmed by an X-ray diffractometer. The coated phosphor powder was characterized by scanning electron microscopy, fluorescence spectrophotometry and contact angle analysis (CAA). The CAA of the phosphor powder coated with the HMDSO precursor revealed that the water contact angle increased from $21.3^{\circ}$ to $139.5^{\circ}$ (max. $148.7^{\circ}$) and the glycerol contact angle from $55^{\circ}$ to $143.5^{\circ}$ (max. $145.3^{\circ}$) as a result of the hydrophobic coating, which indicated that hydrophobic layers were successfully formed on the phosphor powder surfaces. Further surface characterizations were performed by Fourier transform infrared spectroscopy and X-ray photoelectron spectrometry, which also evidenced the formation of hydrophobic coating layers. The phosphor coated with HMDSO exhibited a photoluminescence (PL) enhancement, but the use of toluene or n-hexane somewhat decreased the PL intensity. The results of this work suggest that the DBD plasma may be a viable method for the preparation of hydrophobic coating layer on phosphor powder.

• Journal of the Korean Electrochemical Society
• /
• v.23 no.2
• /
• pp.25-38
• /
• 2020

Photoelectrochemical water splitting has been considered as the most promising technology for generating hydrogen energy. Transition metal dichalcogenide (TMD) compounds have currently attracted tremendous attention due to their outstanding ability towards the catalytic water-splitting hydrogen evolution reaction (HER). Herein, we report the synthesis method of various transition metal dichalcogenide including MoS₂, MoSe₂, WS₂, and WSe₂ nanosheets as excellent catalysts for solar-driven photoelectrochemical (PEC) hydrogen evolution. Photocathodes were fabricated by growing the nanosheets directly onto Si nanowire (NW) arrays, with a thickness of 20 nm. The metal ion layers were formed by soaking the metal chloride ethanol solution and subsequent sulfurization or selenization produced the transition metal chalcogenide. They all exhibit excellent PEC performance in 0.5 M H₂SO₄; the photocurrent reaches to 20 mA cm^-2 (at 0 V vs. RHE) and the onset potential is 0.2 V under AM1.5 condition. The quantum efficiency of hydrogen generation is avg. 90%. The stability of MoS₂ and MoSe₂ is 90% for 3h, which is higher than that (80%) of WS₂ and WSe₂. Detailed structure analysis using X-ray photoelectron spectroscopy for before/after HER reveals that the Si-WS₂ and Si-WSe₂ experience more oxidation of Si NWs than Si-MoS₂ and Si-MoSe₂. This can be explained by the less protection of Si NW surface by their flake shape morphology. The high catalytic activity of TMDs should be the main cause of this enhanced PEC performance, promising efficient water-splitting Si-based PEC cells.

• Journal of Periodontal and Implant Science
• /
• v.33 no.1
• /
• pp.27-35
• /
• 2003

1. 목적 생체재료의 생체친화성을 증진시키고 치유를 촉진하기 위한 목적으로 생체재료의 생화학적 표면개질에 관한 연구가 널리 진행되고 있다. 이와 같은 목적으로 이용되어 온 부착분자에는 아미노산, 펩타이드, 단백질, 효소 및 성장인자들을 들 수 있으며, 이들 분자들을 금속, 골대체물질 및 폴리머와 같은 생체재료의 표면개질에 이용하여 왔다. 이 연구의 목적은 생체적합성이 우수하고 생분해성을 지닌 키토산으로 얇은 막을 제작한 후, 세포외 기질의 구성성분 중 세포부착에 관여하는 RGD 펩타이드를 부착시킨, 표면개질 키토산막의 생물학적 영향을 MG-63 조골양세포를 이용하여 관찰하는 것이다. 2. 방법 2% acetic acid에 키토산 가루를 녹여 만든 2% 키토산 용액으로 24-well 배양접시의 표면을 도포 후 24시간 동안 건조시켜 키토산막을 제작하였다. GRGDS 펩타이드를 cross-linker(EDC, NHS) (Sigma, MO, USA) 용액과 반응시켜서 펩타이드의 카르복실기를 활성화시켰다. 이들을 PBS 완충용액으로 수화시킨 키토산막과 결합시켜 펩타이드의 활성화된 카르복실기와 키토산의 아민기 간에 안정적인 아미드 결합(amide bond)이 형성되도록 하였다. 하루 동안 반응을 일으킨 후 PBS 완충용액과 증류수로 씻어내고 냉동 건조시킴으로써 GRGDS가 결합된 키토산막을 제작하였다. 재료 표면의 화학 성분을 알아보는데 사용되는 방법의 일종인 X-ray photoelectron spectroscopy(XPS) 분석을 통하여 부착분자가 키토산막에 결합된 여부를 확인하였다. GRGDS 펩타이드에 요오드를 결합시킨 후, 이것을 키토산막에 공유 결합시키고 XPS를 통해 요오드가 재료 표면에서 검출되는지를 검사하였다. 요오드가 검출된다면 이것은 키토산막 표면에 실제로 GRGDS 펩타이드가 존재하는 것을 의미하게 된다. 표면개질된 키토산막에 사람조골양세포인 MG-63을 접종하여 이를 실험군으로 하였고, 표면이 개질 되지 않은 키토산막을 대조군으로 하였다. 세포부착의 최적화 농도를 확인하기 위하여 GRGDS를 0.01, 0.05, 0.1, 0.25, 0.5, 1.0mg/ml의 농도로 준비하였다. 배양 후 1일, 7일째에 각 well에서 trypsin EDTA를 이용하여 세포를 분리한 후, 이를 원심 분리하여 세포수측정기를 이용하여 부착 세포의 수를 측정하여 세포의 부착 정도를 비교하였다. 배양 2시간, 24시간 후 주사전자현미경을 이용하여 키토산막에 부착된 세포의 양상을 관찰하였다. 3. 결과 XPS를 통한 표면의 화학 성분 분석 결과 GRGDS 펩타이드를 결합시킨 키토산막에서 요오드가 검출되었으며 펩타이드를 부착하지 않은 대조군에서는 검출되지 않았다. 따라서 cross-linker를 이용한 펩타이드와 키토산막의 공유결합을 확인할 수 있었다. 세포 배양 후 1일째 부착된 세포 수를 측정한 결과 0.1mg/ml 이상의 GRGDS 펩타이드 농도로 공유 결합시킨 키토산막에서 부착 세포 수가 다른 농도에 비해 유의성 있게 많이 관찰되었다. 이 농도 이하에서는 대조군과 실험군간에 세포부착의 유의한 차이가 없었다. 따라서 주사전자현미경을 이용한 부착 세포의 양상에 관한 관찰은 0.1mg/ml 농도의 펩타이드를 이용하였다. 세포 배양 7일째, 부착된 세포 수 측정 결과 GRGDS의 농도에 따른 유의성 있는 차이가 없었으며, 실험군과 대조군간에도 유의성 있는 차이가 없었다. 주사전자현미경 관찰결과 2시간 및 24시간 배양된 실험군 모두에서 별모양의 세포들이 키토산막 표면에 편평하게 잘 부착되어 있으며 많은 위족이 발달된 소견을 보인 반면, 대조군에서는 원형 또는 다각형 모양의 세포들이 실험군에 비해 부착이 덜 되어있는 양상을 보였다. 이 연구를 통하여 기능성 펩타이드를 생체재료의 표면에 공유결합 시키는 방법을 확립할 수 있었으며, RGD 펩타이드의 공유결합으로 표면개질된 키토산막이 조골세포의 부착능을 증진시킬 수 있음을 확인하였다. 표면개질된 생체재료를 소, 중동물에 적용시켜 생체 내에서의 생물학적 영향을 평가할 필요가 있으며, 이 실험의 결과는 향후 다양한 기능성 부착분자를 선발, 고안하여 임플란트용 생체재료의 표면개질에 이용하는 이른바 모방생체재료분야에 널리 활용될 수 있을 것으로 생각된다.

• Applied Chemistry for Engineering
• /
• v.10 no.4
• /
• pp.557-562
• /
• 1999

The reaction properties of Pd. Pd-Ce and Pd-La catalysts supported on ${\gamma}-Al_2O_3$ were investigated in the oxidation reaction of methane($CH_4$) exhausted from the compressed natural gas vehicle in a U-tube flow reactor with gas hourly space velocity of $72,000h^{-1}$. The catalysts were characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), BET surface area and hydrogen chemisorption. Pd catalyst prepared by $Pd(NO_3)_2$ as a palladium precursor and calcined at $600^{\circ}C$ showed the highest activity for a methane oxidation. Catalytic activity of calcined $Pd/{\gamma}-Al_2O_3$ in which most of palladium was converted into palladium oxide species was higher than that of reduced $Pd/{\gamma}-Al_2O_3$ in which most of palladium existed in palladium metal by XRD. As increasing the number of reaction cycles in the wide range of redox, the catalytic activity of $Pd/{\gamma}-Al_2O_3$ was decreased and the highly active window became narrower. Lanthanum oxide promoted Pd catalyst, $Pd/La/{\gamma}-Al_2O_3$ showed enhanced thermal stability compared with $Pd/{\gamma}-Al_2O_3$ even after aging at $1000^{\circ}C$, which was ascribed to the role of La as a promoter to suppress the sintering of palladium metal and ${\gamma}-Al_2O_3$ support. Almost all of methane was removed by the reaction with NO at the redox ratio of 1.2 in case of oxygen excluded steam, but that activity was significantly decreased in the steam containing oxygen.

• Journal of the Korean Chemical Society
• /
• v.47 no.6
• /
• pp.614-618
• /
• 2003

$Sr_2Ru_{1-x}Cu_xO_{4-y}(0.0{\le}x{\le}0.5)$ compounds were prepared using a conventional solid state reaction. Based on the Rietveld refinements of X-ray diffraction results, it is revealed that $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds are the single phases with K2NiF4 type tetragonal system in the range of 0=x=0.3, while the mixed phases of$Sr_2RuO_4$ and $Sr_2CuO_3$ in the range of $0.4{\le}x{\le}0.5$. By means of X-ray photoelectron spectroscopy, the valence states of Ru and Cu in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, have been confirmed to 4+ and 2+, respectively. The bond length difference between $Ru-O_1 ({\times}4)\;and\;Ru-O_2 ({\times}2)\;in\;RuO_6$ octahedron is gradually decreased with increasing Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$, which results in the lower c/a ratio. So, it might be assured that the variation of local symmetry of $RuO_6$ octahedron is very closely related to the transporting property of $Sr_2Ru_{1-x}Cu_xO_{4-y}$ compounds. The behavior of resistivity discloses that the metallic property in $Sr_2RuO_4$ changes into the semiconducting one in proportion to the Cu content in $Sr_2Ru_{1-x}Cu_xO_{4-y}$.

• Korean Journal of Materials Research
• /
• v.8 no.12
• /
• pp.1158-1164
• /
• 1998

Aluminium sulfate solution was prepared by sulfuric acid treatment from gibbsite. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was precipitated from aluminium sulfate solution by adding it into ethylalcohol. From XRD analysis as-prepared $Al_2(SO_4)_3$ · $nH_2O$ was confirmed to have mixed-crystalization water(n=18, 16, 12, 6). The average water of crystalization calculated from thermogravimetry(TG) was 14.7. Aluminium sulfate hydrate [$Al_2(SO_4)_3$ · $nH_2O$] was thermally decomposed and converted to $Al_2(SO_4)_3$ at $800^{\circ}C$, $\gamma-Al_2O_3$ at $900-1000^{\circ}C$, and $\alpha-Al_2O_3$ at $1200^{\circ}C$. Ni-doped $\gamma-Al_2O_3$, was synthesized from the slurry of as-prepared $\gamma-Al_2O_3$, with the ratio of [Ni]/[Al]=0.5. The reaction conditions of synthesis were determined as initial pH 9.0 and temperature $80^{\circ}C$ The basicity(pH) of slurry was controlled by using urea and $NH_4OH$ solution. Urea was also used for deposition-precipitation. For determining termination of reaction, the data acquisition was performed by oxidation reduction potential(ORP), conductivity and pH value in the process of reaction. Termination of the reaction was decided by observing the reaction steps and rapid decrease in conductivity. On the other hand, BET(Brunauer, Emmett and Teller) and thermal diffusity of Ni- doped $\gamma-Al_2O_3$, with various content of Ni were measured and compared. Thermal stability of Ni- doped $\gamma-Al_2O_3$ at $1250^{\circ}C$ was confirmed from BET and XRD analysis. The surface state of Ni-doped $\gamma-Al_2O_3$ was investigated by X-ray photoelectron spectroscopy(XPS). The binding energy at $Ni2P_{3/2}$ increased with increasing the formation of $NiAl_2O_4$ phase.

• Korean Chemical Engineering Research
• /
• v.51 no.5
• /
• pp.609-614
• /
• 2013

This study investigated the spontaneous combustion behavior of solvent-treated low rank coals. Indonesian lignite (a KBB and SM coal) and sub-bituminous (a Roto coal) were mixed with non-polar 1-methyl naphthalene (1MN) either by mechanical agitation or ultrasonication. The property change associated with 1MN treatment was then analyzed using proximate analysis, calorific value analysis, Fourier transform infrared (FT-IR), X-ray photoelectron spectroscopy and moisture re-adsorption test. Susceptibility to spontaneous combustion was evaluated using crossingpoint temperature (CPT) measurement along with gas analysis by GC. A FT-IR profile showed that oxygen functional groups and C-H bonding became weaker when treated by 1 MN. XPS results also indicated a decrease of the oxygen groups (C-O-, C=O and COO-). Increased hydrophobicity was found in the 1MN treated coals during moisture readsorption test. A CPT of the treated coals was ${\sim}20^{\circ}C$ higher than that of the corresponding raw coals and the ultrasonication was more effective way to enhance the stability against spontaneous combustion than the agitation. In the gas analysis less CO and $CO_2$ were emitted from 1MN treated coals, also indicating inhibition of pyrophoric behavior. The surface functional groups participating in the oxidation reaction seemed to be removed by the ultrasonication more effectively than by the simple mechanical agitation.