• Title/Summary/Keyword: XPS (X-ray Photoelectron Spectroscopy)

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Characteristics of Silicon Oxide Thin Films Prepared by Atomic Layer Deposition Using Alternating Exposures of SiH2Cl2 and O3 (SiH2Cl2 와 O3을 이용한 원자층 증착법에 의해 제조된 실리콘 산화막의 특성)

  • Lee Won-Jun;Lee Joo-Hyeon;Han Chang-Hee;Kim Un-Jung;Lee Youn-Seung;Rha Sa-Kyun
    • Korean Journal of Materials Research
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    • v.14 no.2
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    • pp.90-93
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    • 2004
  • Silicon dioxide thin films were deposited on p-type Si (100) substrates by atomic layer deposition (ALD) method using alternating exposures of $SiH_2$$Cl_2$ and $O_3$ at $300^{\circ}C$. $O_3$ was generated by corona discharge inside the delivery line of $O_2$. The oxide film was deposited mainly from $O_3$ not from $O_2$, because the deposited film was not observed without corona discharge under the same process conditions. The growth rate of the deposited films increased linearly with increasing the exposures of $SiH_2$$Cl_2$ and $O_3$ simultaneously, and was saturated at approximately 0.35 nm/cycle with the reactant exposures over $3.6 ${\times}$ 10^{9}$ /L. At a fixed $SiH_2$$Cl_2$ exposure of $1.2 ${\times}$ 10^{9}$L, growth rate increased with $O_3$ exposure and was saturated at approximately 0.28 nm/cycle with $O_3$ exposures over$ 2.4 ${\times}$ 10^{9}$ L. The composition of the deposited film also varied with the exposure of $O_3$. The [O]/[Si] ratio gradually increased up to 2 with increasing the exposure of $O_3$. Finally, the characteristics of ALD films were compared with those of the silicon oxide films deposited by conventional chemical vapor deposition (CVD) methods. The silicon oxide film prepared by ALD at $300^{\circ}C$ showed better stoichiometry and wet etch rate than those of the silicon oxide films deposited by low-pressure CVD (LPCVD) and atmospheric-pressure CVD (APCVD) at the deposition temperatures ranging from 400 to $800^{\circ}C$.

Effects of Thermal and Electrical Conductivity of Al(OH)3 Functionalized Graphene/Epoxy Composites by Simple Sol-Gel Method (졸-젤 법을 이용한 Al(OH)3 처리된 그래핀/에폭시 복합체의 열 및 전기전도 특성 분석)

  • Kim, Ji-Won;Im, Hyun-Gu;Han, Jung-Geun;Kim, Joo-Heon
    • Polymer(Korea)
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    • v.36 no.1
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    • pp.22-28
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    • 2012
  • Functionalized graphene/epoxy composites were prepared to miprove thermal conductivities of epoxy composites and to maintain electrical insulating property. Graphene oxide (GO) was prepared using Hummers method, and then GO was reacted with aluminum isopropoxide to functionalize $Al(OH)_3$ layer onto GO surface by a simple sol-gel method (Al-GO). GO and Al-GO were characterized by X-ray photoelectron spectroscopy, field emission scanning electron microscopy and transmission electron microscopy. The analyses confirm that GO was coated with a large and dense coverage of $Al(OH)_3$. GO and Al-GO (1 and 3 wt%) were embedded in bisphenol A (DGEBA) to investigate the effects of electrical insulating property. Electrical resistivity showed that Al-GO had better insulating property than GO. Further, the thermal conductivity of GO and Al-GO/epoxy composites was higher than that of neat epoxy resins. In particular, the thermal conductivity of Al-GO/bisphenol F (DGEBF) improved by 23.3% and Al-GO/DGEBA enhanced by 21.8% compared with pure epoxy resins.

High Thermoluminescence Properties of Dy+Ce, and Dy+Na Co-Doped MgB4O7 for a Light Tracer Application (비화공식 예광탄 응용을 위한 Dy+Ce 및 Dy+Na 이중 도핑된 MgB4O7의 높은 열발광 특성)

  • Jinu Park;Nakyung Kim;Jiwoon Choi;Youngseung Choi;Sanghyuk Ryu;Sung-Jin Yang;Duck Hyeong Jung;Byungha Shin
    • Korean Journal of Materials Research
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    • v.33 no.1
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    • pp.15-20
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    • 2023
  • 'Tracers' are bullets that emit light at the backside so that the shooter can see the trajectory of their flight. These light-emitting bullets allow snipers to hit targets faster and more accurately. Conventional tracers are all combustion type which use the heat generated upon ignition. However, the conventional tracer has a fire risk at the impact site due to the residual flame and has a by-product that can contaminate the inside of the gun and lead to firearm failure. To resolve these problems, it is necessary to develop non-combustion-type tracers that can convert heat to luminance, so-called 'thermoluminescence (TL)'. Here, we highly improve the thermoluminescence properties of MgB4O7 through co-doping of Dy3++Ce3+ and Dy3++Na+. The presence of doping materials (Dy3+, Ce3+, Na+) was confirmed by XPS (X-ray photoelectron spectroscopy). The as-synthesized co-doped MgB4O7 was irradiated with a specific radiation dose and heated to 500 ℃under dark conditions. Different thermoluminescence characteristics were exhibited depending on the type or amounts of doping elements, and the highest luminance of 370 cd/m2 was obtained when Dy 10 % and Na 5 % were co-doped.

Surface Characteristics and Spontaneous Combustibility of Coal Treated with Non-polar Solvent under Room Temperature (상온에서의 용매 처리를 통한 저등급 석탄의 표면물성 및 자연발화 특성 변화)

  • Jo, Wan Taek;Choi, Ho Kyung;Kim, Sang Do;Yoo, Ji Ho;Chun, Dong Hyuk;Rhim, Young Joon;Lim, Jeong Hwan;Lee, Si Hyun
    • Korean Chemical Engineering Research
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    • v.51 no.5
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    • pp.609-614
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    • 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.

Preparation of Ni-doped Gamma Alumina from Gibbsite and Its Characteristics (깁사이트로부터 니켈피착 감마알루미나의 제조 및 특성)

  • Lee, Hyun;Chung, In-Sung;Park, Hee-Chan
    • Korean Journal of Materials Research
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    • v.8 no.12
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    • pp.1158-1164
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    • 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.

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Development of RGD peptides grafted onto chitosan surfaces; Osteoblast interactions (RGD 펩타이드로 표면개질된 키토산막의 생물학적 영향)

  • Lee, Chang-Kyun;Hwang, Jeong-Hyo;Lee, Yong-Moo;Ku, Young;Rhyu, In-Chul;Lee, Seung-Jin;Han, Soo-Boo;Choi, Sang-Mook;Chung, Chong-Pyoung
    • Journal of Periodontal and Implant Science
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    • v.33 no.1
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    • pp.27-35
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    • 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.