• 한국결정성장학회지
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• 제29권2호
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• pp.45-49
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• 2019

본 연구에서는, 탄소성분으로서 탄화왕겨, 제지슬러지, 커피찌꺼기와 실리카 분말로부터, 비교적 미세한 탄화규소 결정질 응집체를 합성하였다. 탄소성분들과 실리카의 혼합물로부터 탄화규소 응집체를 얻기 위한 주요 반응물질은 열탄화환원 반응에 의해 생성된 일산화규소 기체로 추정되었다. 탄화왕겨, 제지슬러지, 커피찌꺼기와 실리카 분말의 혼합물로부터 열탄화환원반응법을 거쳐 생성된 탄화규소 결정질 응집체들에 대한 XRD 회절패턴으로부터 결정상을 분석하였고, FE-SEM과 FE-TEM을 통한 미세구조, 결정구조 분석이 이루어졌다. 탄화왕겨, 제지슬러지, 그리고 실리카 분말의 시료의 경우, XRD 분석에서는 $35^{\circ}$ 부근의 (111) peak은 비교적 높은 강도를 나타내었다. 탄화왕겨, 제지슬러지, 커피찌꺼기와 실리카 분말의 혼합물로부터 합성된 시료들에 대해 FE-SEM 관찰을 통하여 $1{\mu}m$ 이하의 미세입자들을 관찰하였으며, TEM 측정 결과에서는 탄화규소 결정질상의 (110) 회절패턴들을 확인하였다.

• 대한화학회지
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• 제56권4호
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• pp.484-490
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• 2012

The tin (IV) oxide nanoparticles are prepared by controlled precipitation method and calcined at temperatures of $200-600^{\circ}C$. The prepared $SnO_2$ nanoparticles characterized by XRD patterns, TEM image, IR and UV-Vis spectra. The XRD patterns and TEM image show the tetragonal structure and spherical morphology for $SnO_2$ nanoparticles, respectively. The photocatalytic activity of the prepared $SnO_2$ nanoparticles studied in degradation reaction of methylene blue (MB). The results show the size of nanoparticles, band-gap energy and photocatalytic activity of $SnO_2$ depends on the calcinations temperature. The $SnO_2$ nanoparticles calcined at $500^{\circ}C$ indicated the highest photoreactivity. Also, the zero-valent tin (ZVT) nanoparticles with tetragonal structure are prepared by a reducing agent and used as a catalyst in degradation of MB. In basic pH of 11, the degradation >95% of MB at time 150 min obtained at presence of ZVT nanoparticles.

• Carbon letters
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• 제8권2호
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• pp.95-100
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• 2007

A series of activated carbons (ACs) were derived from sugarcane bagasse under two activation schemes: steam-pyrolysis at $600-800^{\circ}C$ and chemical activation with $H_3PO_4$ at $500^{\circ}C$. Some carbons were treated at 400, $600^{\circ}C$, or for 1-3 h, and/or in flowing air during pyrolysis of acid-impregnated mass. XRD profiles displayed two broad diffuse bands centered around $2{\theta}=23$ and $43^{\circ}$, currently associated with diffraction from the 002 and 100/101 set of planes in graphite, respectively. These correspond to the interlayer spacing, Lc, and microcrystallite lateral dimensions, La, of the turbostratic (fully disordered) graphene layers. Steam pyrolysis-activated carbons exhibit only the two mentioned broad bands with enhancement in number of layers, with temperature, and small decrease in microcrystallite diameter, La. XRD patterns of $H_3PO_4$-ACs display more developed and separated peaks in the early region with maxima at $2{\theta}=23$, 26 and $29^{\circ}$, possibly ascribed to fragmented microcrystallites (or partially organized structures). Diffraction within the $2{\theta}=43^{\circ}$ is still broad although depressed and diffuse, suggesting that the intragraphitic layers are less developed. Varying the conditions of chemical activation inflicts insignificant structural alterations. Circulating air during pyrolysis leads to enhancement of the basic graphitic structure with destruction and degradation in the lateral dimensions.

• 한국재료학회지
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• 제2권2호
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• pp.151-156
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• 1992

본 연구에서는 $Ba(OH)_2{\cdot}8H_2O,\;Sr(OH)_2{\cdot}8H_2O$ 및 $Ti(i-OC_3H_7)_4$를 사용하여 졸-겔법에 의해 미세한 $(Ba_{1-x}Sr_{x})TiO_3$ 분말을 제조하였다. TEM 관찰, BET 비표면적측정 및 XRD회절도의 분석결과 $700^{\cric}C$에서 하소한 뚠말의 입자크기는 20~40nm이고 입방정상으로 존재하였다. 또한 XRD 회절도고부터 계산된 격자상수 및 (112)피크의 이동으로부터 고용체분말이 형성되었음을 확인할 수 있었다. 제조된 분말에서의 EDAX 분석을 통한 양이온들의 상대적인 비율 및 소결체에 대한 유전상수의 측정결과로부터 제조된 분말에서 양이온들의 분포가 입자단위에서 균질함을 예상할 수 있었다.

• 한국분말재료학회지
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• 제23권2호
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• pp.136-142
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• 2016

As precursors of cathode materials for lithium ion batteries, $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$ powders are prepared in a continuously stirred tank reactor via a co-precipitation reaction between aqueous metal sulfates and NaOH in the presence of $NH_4OH$ in air or nitrogen ambient. Calcination of the precursors with $Li_2CO_3$ for 8 h at $1,000^{\circ}C$ in air produces dense spherical cathode materials. The precursors and final powders are characterized by X-ray diffraction (XRD), scanning electron microscopy, particle size analysis, tap density measurement, and thermal gravimetric analysis. The precursor powders obtained in air or nitrogen ambient show XRD patterns identified as $Ni_{1/3}Co_{1/3}Mn_{1/3}(OH)_2$. Regardless of the atmosphere, the final powders exhibit the XRD patterns of $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ (NCM). The precursor powders obtained in air have larger particle size and lower tap density than those obtained in nitrogen ambient. NCM powders show similar tendencies in terms of particle size and tap density. Electrochemical characterization is performed after fabricating a coin cell using NCM as the cathode and Li metal as the anode. The NCM powders from the precursors obtained in air and those from the precursors obtained in nitrogen have similar initial charge/discharge capacities and cycle life. In conclusion, the powders co-precipitated in air can be utilized as precursor materials, replacing those synthesized in the presence of nitrogen injection, which is the usual industrial practice.

• 한국분말재료학회지
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• 제21권3호
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• pp.207-214
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• 2014

In this study, nano-scale copper powders were reduction treated in a hydrogen atmosphere at the relatively high temperature of $350^{\circ}C$ in order to eliminate surface oxide layers, which are the main obstacles for fabricating a nano/ultrafine grained bulk parts from the nano-scale powders. The changes in composition and microstructure before and after the hydrogen reduction treatment were evaluated by analyzing X-ray diffraction (XRD) line profile patterns using the convolutional multiple whole profile (CMWP) procedure. In order to confirm the result from the XRD line profile analysis, transmitted electron microscope observations were performed on the specimen of the hydrogen reduction treated powders fabricated using a focused ion beam process. A quasi-statically compacted specimen from the nano-scale powders was produced and Vickers micro-hardness was measured to verify the potential of the powders as the basis for a bulk nano/ultrafine grained material. Although the bonding between particles and the growth in size of the particles occurred, crystallites retained their nano-scale size evaluated using the XRD results. The hardness results demonstrate the usefulness of the powders for a nano/ultrafine grained material, once a good consolidation of powders is achieved.

• Carbon letters
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• 제21권
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• pp.33-50
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• 2017

In this study, Fe-Ni bimetallic catalyst supported on kaolin is prepared by a wet impregnation method. The effects of mass of kaolin support, pre-calcination time, pre-calcination temperature and stirring speed on catalyst yields are examined. Then, the optimal supported Fe-Ni catalyst is utilised to produce multi-walled carbon nanotubes (MWCNTs) using catalytic chemical vapour deposition (CCVD) method. The catalysts and MWCNTs prepared using the optimal conditions are characterized using high resolution transmission electron microscope (HRTEM), high-resolution scanning electron microscope (HRSEM), electron diffraction spectrometer (EDS), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and X-ray diffraction (XRD). The XRD/EDS patterns of the prepared catalyst confirm the formation of a purely crystalline ternary oxide ($NiFe_2O_4$). The statistical analysis of the variance demonstrates that the combined effects of the reaction temperature and acetylene flow rate predominantly influenced the MWCNT yield. The $N_2$ adsorption (BET) and TGA analyses reveal high surface areas and thermally stable MWCNTs. The HRTEM/HRSEM micrographs confirm the formation of tangled MWCNTs with a particle size of less than 62 nm. The XRD patterns of the MWCNTs reveal the formation of a typical graphitized carbon. This study establishes the production of MWCNTs from a bi-metallic catalyst supported on kaolin.

• 한국자기학회지
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• 제23권1호
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• pp.12-17
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• 2013

금속 분말 니켈(Ni)을 HCl용액에 용해시킨 후 $H_3BO_3$, KOH을 첨가하여 Chloride 도금용액을 제조 후 Ni plate 기판에 도금하였다. 도금두께는 $3{\mu}m$로 일정하게 유지하였다. 전류밀도를 $1{\sim}30mA/cm^2$ 변화를 준 결과 전류밀도를 증가시킬수록 Ni 후막표면이 거칠어졌다. $25mA/cm^2$와 $30mA/cm^2$에서는 균열된 표면형상을 관찰하였다. 또한 XRD patterns 변화를 관찰한 결과 전류밀도가 증가할수록 FCC(111)과 FCC(220) 및 FCC(311)상의 강도는 증가한 반면 FCC(200)상의 강도는 감소하는 것을 관찰하였다. 전기도금된 Ni의 수평 및 수직 자화 값을 측정하였는데 기판에 의한 수평자화 값이 크게 나왔고, 코팅층 두께가 증가할수록 수직자화 값이 커지는 것을 확인하였다.

• 한국분말재료학회지
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• 제19권5호
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• pp.343-347
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• 2012

In this study, an oxygen plasma treatment was used as a low temperature debinding method to form a conductive copper feature on a flexible substrate using a direct printing process. To demonstrate this concept, conductive copper patterns were formed on polyimide films using a copper nanoparticle-based paste with polymeric binders and dispersing agents and a screen printing method. Thermal and oxygen plasma treatments were utilized to remove the polymeric vehicle before a sintering of copper nanoparticles. The effect of the debinding methods on the phase, microstructure and electrical conductivity of the screen-printed patterns was systematically investigated by FE-SEM, TGA, XRD and four-point probe analysis. The patterns formed using oxygen plasma debinding showed the well-developed microstructure and the superior electrical conductivity compared with those of using thermal debinding.

• 한국세라믹학회지
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• 제35권10호
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• pp.1113-1119
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• 1998

Crystal structure of needle-shaped maghemite(${\gamma}$-{{{{ { {Fe }_{2 }O }_{3 } }}) has been studied by the Rieveld analysis of powder X-ray diffraction patterns. The tetragonal space group P41,.3212 and cubic space group P41,.32 have been have been used for the refinement of X-ray diffraction patterns. The crystal system of maghemite is closed to tetragonal more than cubic. The tetragonal lattice parameters are a=8.3460$\AA$ and c=25.034$\AA$ The standard X-ray diffraction pattern of the tetragonal maghemite analyzed with space group P41,.3212 is proposed.