• Carbon letters
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• 제21권
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• pp.51-60
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• 2017

Isotropic pitch-based fibers produced from coal tar pitch with the melt-blowing method were carbonized at temperatures ranging from 800 to $1600^{\circ}C$ to investigate their crystalline structure and physical properties as a function of the carbonization temperature. The in-plane crystallite size ($L_a$) of the carbonized pitch fiber from X-ray diffraction increased monotonously by increasing the carbonization temperature resulting in a gradual increase in the electrical conductivity from 169 to 3800 S/cm. However, the variation in the $d_{002}$ spacing and stacking height of the crystallite ($L_c$) showed that the structural order perpendicular to the graphene planes got worse in carbonization temperatures from 800 to $1200^{\circ}C$ probably due to randomization through the process of gas evolution; however, structural ordering eventually occurred at around $1400^{\circ}C$. For the carbonized pitch powder without stabilization, structural ordering perpendicular to the graphene planes occurred at around $800-900^{\circ}C$ indicating that oxygen was inserted during the stabilization process. Additionally, the shear stress that occurred during the melt-blowing process might interfere with the crystallization of the CPF.

• 한국세라믹학회지
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• 제28권11호
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• pp.926-934
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• 1991

The effect of aggregates on the forming and sintering behaviors of BaTiO3 was studied. Aggregates and deaggregates of fine crystallite were obtained by thermal decomposition of oxalate coprecipitates and subsequently crushing them with a press, respectively. Large voids formed by packing of aggregates were not easily eliminated despite the successive destruction of aggregates with increasing forming pressure. As a result, compacts of aggregates showed inhomogeneity with larger mid-pore size and broader pore size distribution with respect to those of deaggregates. This inhomogeneity caused differential shrinkage and consequental internal stress, which retarded densification. The differential sintering increased the size of mid-pores in the initial stage, and formed duplex structure composed of dense region with abnormally grown grains and porous region with fine grains. The driving force of this abnormal grain growth shown in the specimens of aggregates was attributed to the minimization of the elastic strain energy due to internal stress.

• 한국결정성장학회지
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• 제27권3호
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• pp.122-129
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• 2017

고밀도 ITO 타겟 제조를 위해 입자의 크기가 미세하면서도 응집성이 적은 $In_2O_3$ 분말을 합성해야 한다. 본 실험에서는 $In_2O_3$ 분말의 특성에 영향을 미치는 전구체 Indium hydroxide 분말의 크기와 형상을 제어하는 것에 목적을 두고 있다. 출발 물질로써 Indium metal을 질산($HNO_3$)과 증류수의 혼합용액에 용해시켜 $In(NO_3)_3$ 용액을 만들었다. 침전제로 수산화암모늄($NH_4OH$)을 사용하여 농도, pH, 온도가 Indium hydroxide 특성에 미치는 영향을 분석하였다. X-ray diffraction으로 각 시료의 결정상을 분석하고 Crystallite size를 계산하였으며, TEM으로 입자의 형상과 크기를 분석하였다. 그 결과 $In(NO_3)_3$ 농도가 증가할수록 얻어지는 Indium hydroxide의 입자크기는 증가하였고 일정한 농도의 $In(NO_3)_3$ 용액에서 침전 pH 변화에 따른 Indium hydroxide의 입자크기와 형상의 변화는 관찰되지 않았다. 침전 시 온도가 상승할수록 입자크기는 증가하였다.

• 한국염색가공학회지
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• 제27권4호
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• pp.245-260
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• 2015

The effect of salt milling process on the crystal size, morphology, and color characteristics of C.I. Pigment Red 57:1 was studied. The primitive morphology and color properties of the pigment after synthesis were studied in the former series work. The size and morphology of primary particles and the second aggregation features should be considered because they are very important to determine pigment quality. We compared the primary morphology of pigment particles before drying with the secondary aggregated morphology of pigment particles after drying and salt milling process. Morphological properties were investigated by particle size analysis, X-ray diffraction, and scanning electron microscopy and color measurement was carried out. Significant reduction in particle size as well as enhanced crystallite size after salt milling process was observed. This result might give a difference in color of the pigment, turning into brighter and more blue-toned red color. It was revealed that synthesis condition affect the morphology and color of the pigment even after milling. Increase in HCl concentration in the synthesis process enhanced crystal size and quality forming bluer-red pigments but an increase in $CaCl_2$ concentration resulted in more amorphous crystals forming darker-red pigments after salt milling.

• 공업화학
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• 제21권4호
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• pp.440-444
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• 2010

$SnCl_4$와 침전제로 ammonium nitrate ($NH_4NO_3$)의 수용액들을 사용하여 $90^{\circ}C$에서 침전반응으로 얻은 주석산(stannic acid)을 열처리하여 $SnO_2$ 분말을 제조하였으며, 요소($(NH_2)_2CO$)를 침전제로 사용한 균일침전법으로 주석산을 제조하여 열처리 전후로 재료의 특성을 상호 비교하였다. Ammonium nitrate의 침전법에 의한 주석산은 열처리에 따른 중량감소가 $700^{\circ}C$까지 이루어졌으며, 전체 중량감소는 16.5%였다. 또한 $600^{\circ}C$의 열처리로 비정질 주석산이 완전한 결정질의 $SnO_2$로 상변화가 이루어졌다. 주석산 제조 과정에서 $SnCl_4$ 수용액의 농도 증가 및 열처리 온도 증가에 따라 $SnO_2$의 결정입계가 증가하였다. 요소를 침전제로 사용한 균일침전법은 ammonium nitrate를 침전제로 하는 균일법보다 같은 조건의 열처리 공정 후에 상대적으로 미세한 결정입계의 $SnO_2$를 얻을 수 있었다.

• 한국결정성장학회지
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• 제18권4호
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• pp.174-178
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• 2008

본 연구에서는 균일침전법으로 합성된 $CaCO_3$를 하소한 후 수화시키는 방법을 이용하여 소석회를 제조하였다. 소석회를 제조하기 위하여, 염화칼슘$(CaCl_2)$과 우레아(Urea)가 출발 물질로 사용되었으며 염화칼슘 수용액과 우레아 수용액을 혼합하여 가열하는 동안 반응용기 내에서 탄산칼슘이 합성되었다. 침전물들을 여과하고 증류수와 에탄올로 수 차례 세척하였으며 건조시켰다. 소석회는 하소된 탄산칼슘의 수화과정을 통하여 합성되었다. 최적의 합성조건을 선정하는데 있어 실험의 잡음인자를 최소화하고 결과를 통계적으로 추론할 수 있는 실험계획법(다구치 실험계획법)을 이용하였다. 제조된 탄산칼슘을 $1000^{\circ}C$에서 30분 동안 하소시킨 후 에탄올 및 옥살산이 첨가된 증류수로 수화시킴으로써 결정입자 크기가 약 50 nm인 소석회를 제조할 수 있었다.

• Journal of Magnetics
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• 제20권3호
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• pp.229-240
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• 2015

In this study, nanocrystalline ferrite powders with the composition $Ni_{0.5}Zn_{0.5}Fe_2O_4$ were prepared by the autocombustion method. The obtained powders were sintered at $800^{\circ}C$, $900^{\circ}C$ and $1,000^{\circ}C$ for 4 h in air atmosphere. The as-prepared and the sintered powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and magnetization studies. An increase in the crystallite size and a slight decrease in the lattice constant with sintering temperature were observed, whereas microstrain was observed to be negative for all the samples. Two significant absorption bands in the wave number range of the $400cm^{-1}$ to $600cm^{-1}$ have been observed in the FT-IR spectra for all samples which is the distinctive feature of the spinel ferrites. The force constants were found to vary with sintering temperature, suggesting a cation redistribution and modification in the unit cell of the spinel. The M-H loops indicate smaller coercivity, which is the typical nature of the soft ferrites. The observed variation in the saturation magnetization and coercivity with sintering temperature has been attributed to the role of surface, inhomogeneous cation distribution, and increase in the crystallite size.

• 한국세라믹학회지
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• 제39권8호
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• pp.764-768
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• 2002

산화물의 금속 전구체인 $Ce(OH)_4$를 희석제인 NaCl과 함께 기계적으로 분쇄하여 나노 크기의 일차입자를 제조하고, 분쇄한 전구체 분말은 희석제와 함께 열처리를 하여 나노 결정립의 $CeO_2$를 합성하였다. 희석제는 전구체의 분쇄시 분말의 재응집을 억제하여 분쇄효율을 증진시켰을 뿐만 아니라 열처리 중에는 일차입자 성장과 응집을 억제하여 열처리 온도와 시간에 따라 일차입자의 크기 뿐만 아니라 응집체으 크기도 제어할 수 있었다. 열처리 중 희석제는 고온에서 전구체 표면에서 치밀화 되어 일차입자 성장과 응집체 형성의 확산장벽으로 작용하는 것으로 판단되며 열처리 후 증류수에 쉽게 용해되어 $CeO_2$ 나노 입자 제조에 효과적이었다. 일차입자와 응집체의 크기 및 결정성은 희석제의 농도, 열처리 온도와 시간에 의존하는 것으로 확인 되었다.

• 한국세라믹학회지
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• 제24권2호
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• pp.123-132
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• 1987

Yttria-stabilized zirconia with erbia-lanthana were investigated with respect to the amount of Ln2O3 (Ln; Er, La) addition in the range of 0.5∼5 mol% to the base composition of 8 mol% yttriazirconia. Following analysis and measurement were adopted for the characterization of synthesizes of solid electrolyte; phase transformation, lattice parameter, crystallite size, relative density, chemical composition and SEM/EDS. Electrical conductivity by two-probe method versus temperature from 350$^{\circ}C$ to 800$^{\circ}C$ and frequency in the range of 5Hz∼13MHz by complex impedance method was also conducted together with the determination of oxygen ion transference number by EMF method for the evaluation of their electrical properties. The results were as followsing; Electrical conductivity were decreased with increase in Ln2O3 content, but their activation energies increased. In the case of La2O3 addition, espicially, its electrical conductivity was decreased owing to the segregation of second phases at the grain-boundary. Grain-boundary conductivity of the specimen contained 0.5 mol% Er2O3 exhibited a maximum conductivity among thecompositions experimented. However, their bulk conductivities decreased in both case. Oxygen ion transference number was also reduced with decrease in oxygen partial pressure. For example, in the case of Er2O3 addition it retained value in the range of 0.97∼0.94 abvove 4.74${\times}$10-2in oxygen partial pressure. With the increase in the quantities of the evaporation of additive components, the crystallite size of stabilized zirconia decreased, and their relative density also reduced owing to the formation of porosity in their matrices. In the case of La2O3 the sinterbility was improved in the limited amount of addition up to 0.5 mol%, in the same range of addition the strength of sintered bodies were improved perhaps owing to the precipitation of metastable tetragonal phase in the fully stabilized zirconia.

• 대한화학회지
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• 제62권2호
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• pp.118-123
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• 2018

The hexagonal tungsten bronze $Cs_xWO_3$ nanoparticle was synthesized by a chemical coprecipitation method of ammonium tungstate and $Cs_2CO_3$ in acidic condition. This synthetic method for cesium tungsten bronze is reported for the first time as far as we know. The synthesized $Cs_xWO_3$ as precipitated showed a weak crystallinity of hexagonal unit cell with a crystallite size of about 4 nm without annealing. When the synthesized $Cs_xWO_3$ was annealed in $N_2$ atmosphere, the crystallinity and crystallite size systematically increased maintaining the typical hexagonal tungsten bronze structure as the annealing temperature increased. The analyzed Cs content in the bronze was about 0.3 vs W, which is very close to the theoretical maximum value, 1/3 in cesium tungsten bronze. According to XPS analysis, the reduced tungsten ions existed as both the forms of $W^{5+}$ and $W^{4+}$ and the contents systematically increased as the annealing temperature increased up to $800^{\circ}C$. The $Cs_xWO_3$ thin films on PET substrate were also prepared by a wet-coating method using the ball-milled solution of the annealed $Cs_xWO_3$ nanoparticles at various temperatures. The near-infrared shielding property of these thin films increased systematically as the annealing temperature increased up to $800^{\circ}C$ as expected with the increased contents of reduced tungsten ions.