• Title/Summary/Keyword: electron spectroscopy for chemical analysis

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Empirical relationship between band gap and synthesis parameters of chemical vapor deposition-synthesized multiwalled carbon nanotubes

  • Obasogie, Oyema E.;Abdulkareem, Ambali S.;Mohammed, Is'haq A.;Bankole, Mercy T.;Tijani, Jimoh. O.;Abubakre, Oladiran K.
    • Carbon letters
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    • v.28
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    • pp.72-80
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    • 2018
  • In this study, an empirical relationship between the energy band gap of multi-walled carbon nanotubes (MWCNTs) and synthesis parameters in a chemical vapor deposition (CVD) reactor using factorial design of experiment was established. A bimetallic (Fe-Ni) catalyst supported on $CaCO_3$ was synthesized via wet impregnation technique and used for MWCNT growth. The effects of synthesis parameters such as temperature, time, acetylene flow rate, and argon carrier gas flow rate on the MWCNTs energy gap, yield, and aspect ratio were investigated. The as-prepared supported bimetallic catalyst and the MWCNTs were characterized for their morphologies, microstructures, elemental composition, thermal profiles and surface areas by high-resolution scanning electron microscope, high resolution transmission electron microscope, energy dispersive X-ray spectroscopy, thermal gravimetry analysis and Brunauer-Emmett-Teller. A regression model was developed to establish the relationship between band gap energy, MWCNTs yield and aspect ratio. The results revealed that the optimum conditions to obtain high yield and quality MWCNTs of 159.9% were: temperature ($700^{\circ}C$), time (55 min), argon flow rate ($230.37mL\;min^{-1}$) and acetylene flow rate ($150mL\;min^{-1}$) respectively. The developed regression models demonstrated that the estimated values for the three response variables; energy gap, yield and aspect ratio, were 0.246 eV, 557.64 and 0.82. The regression models showed that the energy band gap, yield, and aspect ratio of the MWCNTs were largely influenced by the synthesis parameters and can be controlled in a CVD reactor.

Fabrication and Characterization of Highly Reactive Al/CuO Nano-composite using Graphene Oxide (산화그래핀을 적용한 고반응성 Al/CuO 나노복합재 제조 및 분석)

  • Lim, YeSeul
    • Journal of Powder Materials
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    • v.26 no.3
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    • pp.220-224
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    • 2019
  • The aluminum (Al)/copper oxide (CuO) complex is known as the most promising material for thermite reactions, releasing a high heat and pressure through ignition or thermal heating. To improve the reaction rate and wettability for handling safety, nanosized primary particles are applied on Al/CuO composite for energetic materials in explosives or propellants. Herein, graphene oxide (GO) is adopted for the Al/CuO composites as the functional supporting materials, preventing a phase-separation between solvent and composites, leading to a significantly enhanced reactivity. The characterizations of Al/CuO decorated on GO(Al/CuO/GO) are performed through scanning electron microscopy, transmission electron microscopy, and energy dispersive X-ray spectroscopy mapping analysis. Moreover, the functional bridging between Al/CuO and GO is suggested by identifying the chemical bonding with GO in X-ray photoelectron spectroscopy analysis. The reactivity of Al/CuO/GO composites is evaluated by comparing the maximum pressure and rate of the pressure increase of Al/CuO and Al/CuO/GO. The composites with a specific concentration of GO (10 wt%) demonstrate a well-dispersed mixture in hexane solution without phase separation.

Preparation and characterization of magnetic nanoparticles with two kinds of core/shell structures (핵/껍질 구조를 가진 두 종류의 자기 나노입자의 제조와 특성비교)

  • 고영재;손인호;김영국;동성용;이근진;박규섭
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.87-92
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    • 2001
  • Magnetic Fe-Co(C) nanocapsules and Fe-Co nanoparticles were prepared by arc-discharge in two kinds of atmospheres, i.e. methane and a mixture of ($H_2$+Ar), respectively. Characterization and magnetic properties of this two kinds of ultrafine particles were investigated systematically by means of X-ray diffraction, Mssbauer spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, energy disperse spectroscopy analysis, chemical analysis, oxygen determination and magnetization measurement. Effects of carbon element, decomposed from a methane atmosphere in carbon arc process, on phase structures, magnetic states and surface characterization were studied in comparison to that of Ar element. Two ultrafine particles showed a little difference in the weight ratio of (Fe/co) and the size for Fe-Co nanoparticles was about two times bigger than Fe-Co(C) nanocapsules. The saturation magnetization of Fe-Co (C) nanocapsules was about 8% higher than that of Fe-Co nanoparticles while their phase constitutions were similar. Although no carbon could be detected by XRD measurement because of extremely thin shells on the surfaces of the cores, it is still believed that they are carbon and oxygen layers.

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Preparation of melamine-grafted graphene oxide and evaluation of its efficacy as a flame retardant additive for polypropylene

  • Monji, Parisa;Jahanmardi, Reza;Mehranpour, Milad
    • Carbon letters
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    • v.27
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    • pp.81-89
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    • 2018
  • The present study aimed to prepare a novel efficient flame retardant additive for polypropylene. The new flame retardant was prepared by chemical grafting of melamine to graphene oxide with the aid of thionyl chloride. Fourier-transform infrared spectroscopy and thermogravimetric analysis proved that melamine had been successfully grafted to the graphene oxide. The modified graphene oxide was incorporated into polypropylene via solution mixing followed by anti-solvent precipitatio. Homogeneous distribution as well as exfoliation of the nanoplatelets in the polymer matrix was observed using transmission electron microscopy. Thermogravimetric analysis showed a significant improvement in the thermo-oxidative stability of the polymer after incorporating 2 wt% of the modified graphene oxide. The modified graphene oxide also enhanced the limiting oxygen index of the polymer. However, the amount of improvement was not enough for the polymer to be ranked as a self-extinguishing material. Cone calorimetry showed that incorporating 2 wt% of the modified graphene oxide lowered total heat release and the average production rate of carbon monoxide during burning of the polymer by as much as 40 and 35%, respectively. Hence, it was concluded that the new flame retardant can retard burning of the polymer efficiently and profoundly reduce suffocation risk of exposure to burning polymer byproducts.

Effect of Electron Beam Irradiation on the Properties of Carbon Fiber (전자선 조사에 따른 탄소섬유 물성 변화)

  • Jeun, Joon Pyo;Shin, Hye-Kyoung;Kim, Hyun Bin;Kang, Phil Hyun
    • Journal of Radiation Industry
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    • v.4 no.3
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    • pp.259-263
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    • 2010
  • Carbon fibers are used as a reinforcement material in an epoxy matrix in advanced composites due to their high mechanical strength, rigidity and low specific density. An important aspect of the mechanical properties of composites is associated to the adhesion between the surface of the carbon fiber and the epoxy matrix. This paper aimed to evaluate the effects of electron beam irradiation on the physicochemical properties of carbon fibers to obtain better adhesion properties in resultant composite. Chemical structure and surface elements of carbon fiber were determined by FT-IR, elemental analysis and X-ray photoelectron spectroscopy, which indicated that the oxygen content increased significantly with increasing the radiation dose. Thermal stability of the carbon fibers was studied via the thermalgravimetric analysis. Surface morphology of carbon fiber was analyzed by scanning electron microscope. It was found that the degree of surface roughness was increased by electron beam irradiation.

Nitrogen-doped carbon nanosheets from polyurethane foams and removal of Cr(VI)

  • Duan, Jiaqi;Zhang, Baohua;Fan, Huailin;Shen, Wenzhong;Qu, Shijie
    • Carbon letters
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    • v.22
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    • pp.60-69
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    • 2017
  • Nitrogen-doped carbon nanosheets with a developed porous structure were prepared from polyurethane foams by hydrothermal carbonization following $ZnCl_2$ chemical activation. Scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, solid state $^{13}C$ nuclear magnetic resonance (NMR) spectra and X-ray photoelectron spectroscopy were used to characterize the nitrogen-doped carbon nanosheet structure and composition. The removal of Cr(VI) by the N-doped carbon nanosheets was investigated. The results showed that the maximum removal capacity for chromium of 188 mg/g was found at pH=2.0 with PHC-Z-3. pH had an important effect on Cr(VI) removal and the optimal pH was 2.0. Moreover, amino groups and carboxyl groups in the nitrogen-doped carbon nanosheet played important roles in Cr(VI) removal, and promoted the reduction of Cr(VI) to Cr(III).

A Study on the Preparation and Purification Characteristics of Graphene Oxide by Graphite Type (흑연 종류에 따른 산화 그래핀의 제조 및 정제를 통한 특성연구)

  • Jeong, Kyeom;Kim, Young-Ho
    • Clean Technology
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    • v.27 no.2
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    • pp.132-138
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    • 2021
  • Research is being conducted on graphene to provide graphene having both excellent physical as well as electrical properties in addition to unique physical properties. In this study, Hummer's method, which is a representative method for chemical exfoliation, was applied in order to investigate the possibility of the mass production of high-quality graphene oxide. Three types of graphite (graphite, crystalline graphite, and expanded graphite) were used in the preparation of graphene oxide with variations in the amount of potassium permanganate added, reaction temperature, and reaction time. Then a Fourier transform infrared spectroscopy (FT-IR), a Raman spectrometer, and a transmission electron microscope (TEM) were used to measure the quality of the prepared graphene oxide. Of the three types of graphite used in this experiment, crystalline graphite showed the highest quality. The prepared graphene oxide was then purified with an organic solvent, and an analysis conducted using energy dispersive X-ray spectroscopy (EDS). From the results of the residual values, we were able to confirm that both acid wastewater and wastewater were best purified using cyclohexane. The method for manufacturing graphene oxide as well as the method of purification using organic solvents that are presented in this study are expected to have less of an environmental impact, making them environmentally friendly. This makes them suitable for use in various industrial fields such as the film industry and for heat dissipation and as coating agents.

Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.

A Study of the Etched ZnO Thin Films Surface by Reactive Ion in the Cl2/BCl3/Ar Plasma (Cl2/BCl3/Ar 플라즈마에서 반응성 이온들에 의해 식각된 ZnO 박막 표면 연구)

  • Woo, Jong-Chang;Kim, Chang-Il
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.23 no.10
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    • pp.747-751
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    • 2010
  • In the study, the characteristics of the etched Zinc oxide (ZnO) thin films surface, the etch rate of ZnO thin film in $Cl_2/BCl_3/Ar$ plasma was investigated. The maximum ZnO etch rate of 53 nm/min was obtained for $Cl_2/BCl_3/Ar$=3:16:4 sccm gas mixture. According to the x-ray diffraction (XRD) and atomic force microscopy (AFM), the etched ZnO thin film was investigated to the chemical reaction of the ZnO surface in $Cl_2/BCl_3/Ar$ plasma. The field emission auger electron spectroscopy (FE-AES) analysis showed an elemental analysis from the etched surfaces. According to the etching time, the ZnO thin film of etched was obtained to The AES depth-profile analysis. We used to atomic force microscopy to determine the roughness of the surface. So, the root mean square of ZnO thin film was 17.02 in $Cl_2/BCl_3/Ar$ plasma. Based on these data, the ion-assisted chemical reaction was proposed as the main etch mechanism for the plasmas.

Pyrolytic Carbon Coating on A Simulated Fuel by Fluidized Bed Type Chemical Vapour Deposition

  • Park, Y.;Kim, Bong G.;Lee, Young W.;Dong S. Sohn
    • Proceedings of the Korean Nuclear Society Conference
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    • 1997.05b
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    • pp.159-164
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    • 1997
  • Pyrolytic carbon layer was coated on A1203 balls by fluidized bed type chemical vapour deposition unit to develop the coating technology for the preparation of coated nuclear fuel. The deposition was carried out at the temperature ranges between 110$0^{\circ}C$ and 130$0^{\circ}C$ with various gas contents and flow rates. Source and carrier gas were propane and argon, respectively. X-ray analysis shows that the deposition layer was typical carbon spectra. The growth rate of carbon layer depended on the amount of source gas and the deposition temperature. For the alumina balls with 2mm in diameter, the deposition rate was 11${\mu}{\textrm}{m}$/hr in the flow gases containing 30% source gas at 130$0^{\circ}C$ with a total flow rate of 2.0$\ell$/min. Microstructural observation of the deposits with scanning electron microscope revealed that the deposits had relatively dense and isotropic structure. Chemical analysis by energy dispersive spectroscopy showed that the layer was pure carbon.

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