• Title/Summary/Keyword: Crystallite Size

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Effect of carbonization temperature on crystalline structure and properties of isotropic pitch-based carbon fiber

  • Kim, Jung Dam;Roh, Jae-Seung;Kim, Myung-Soo
    • Carbon letters
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    • v.21
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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.

Effect of Aggregates on the Sintering Behavior of $BaTiO_3$ (응집입자가 $BaTiO_3$의 소결거동에 미치는 영향)

  • 김진호
    • Journal of the Korean Ceramic Society
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    • v.28 no.11
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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.

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Synthesis of indium hydroxide powders by a precipitation method (침전법을 이용한 Indium hydroxide 분말의 합성 연구)

  • Choi, Eun-Kyoung;Lee, Won-Jun;Han, Kyu-Sung;Kim, Ung-Soo;Kim, Jin-Ho;Hwang, Kwang-Teak;Kim, Jong-Young;Hwang, Hae-Jin;Shim, Kwang-Bo;Cho, Woo-Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.3
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    • pp.122-129
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    • 2017
  • For the production of a high-density ITO target, $In_2O_3$ powders with a small particle size and low agglomeration should be synthesized. The purpose of this study is to control the size and shape of the Indium hydroxide precursor which affects the properties of the $In_2O_3$ powder. As a starting raw material, Indium metal was dissolved in a Nitric acid ($HNO_3$) solution. The effect of concentration, pH, and temperature on the properties of Indium hydroxide was investigated using ammonium hydroxide as a precipitant. Crystallite size of each sample was analyzed by X-ray diffraction and the shape and the size of the powder was analyzed by transmission electron microscopy. As a result, the particle size of Indium hydroxide was increased with increase in the concentration of $In(NO_3)_3$ and the particle size and shape of the Indium hydroxide remained unchanged with increase in the pH of the solution. The particle size increased with increase in the precipitation temperature during precipitation.

Particle Size, Morphology and Color Characteristics of C.I. Pigment Red 57:1 : 2. Effect of Salt Milling Process

  • Seo, Hee Sung;Lee, Hyun Kyung;Yoo, Eui Sang
    • Textile Coloration and Finishing
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    • v.27 no.4
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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.

Characteristics of $SnO_2$ Prepared by Preparation Method with Ammonium Nitrate (Ammonium Nitrate를 이용한 침전법으로 제조된 $SnO_2$ 특성분석)

  • Son, Hyang-Ho;Lee, Won-Gyu
    • Applied Chemistry for Engineering
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    • v.21 no.4
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    • pp.440-444
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    • 2010
  • $SnO_2$ powders were prepared from the calcination of stannic acids precipitated from the aqueous solution of $SnCl_4$ with ammonium nitrate as a precipitator at $90^{\circ}C$. For the comparison of properties, the stannic acids were prepared from the homogeneous precipitation method using urea as a precipitator at the same temperature. The stannic acid from ammonium nitrate at a thermal gravity analysis showed the weight loss until $700^{\circ}C$ and the percentage of total weight loss was 16.5%. The crystallization of stannic acid into $SnO_2$ finished in the calcination at $600^{\circ}C$ for 2 h. The crystallite size of $SnO_2$ increased with the increase of calcination temperature and initial concentration of $SnCl_4$ solution. In case of the same calcination condition, $SnO_2$ prepared from homogeneous precipitation using urea had a relatively smaller crystallite size rather than $SnO_2$ prepared from ammonium nitrate.

Synthesis of nano-crystalline slaked lime using design of experiment (실험계획법을 이용한 나노 결정 소석회 합성)

  • Kim, Jin-Seong;Kim, Jung-Woo;Lee, Hee-Soo;Kim, Yong-Nam;Shin, Hyun-Gyoo;Kim, Hwan
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.4
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    • pp.174-178
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    • 2008
  • Nano-crystalline slaked lime was synthesized using design of experiment. In order to synthesize slaked lime, calcium chloride $(CaCl_2)$ and urea were used as starting materials. Calcium chloride solution and urea solution were mixed and heated in vessel that calcium carbonate was precipitated during heating. Precipitates were filtered, washed several times using D.I.water and ethanol and finally dried in oven. Slaked lime $(Ca(OH)_2)$ has been fabricated by the hydration of calcined $CaCO_3$. Design of experiment (Taguchi method) was used to optimize parameter, to minimize noise factors of experiment and to statistically analyze the results. Slaked lime having about 50 nm in optimized crystallite size could be obtained by calcination of $CaCO_3$ at $1000^{\circ}C$ for 0.5 h and hydration with D.I water containing ethanol and oxalic acid.

Effect of Sintering Temperature on the Micro Strain and Magnetic Properties of Ni-Zn Nanoferrites

  • Venkatesh, D.;Siva Ram Prasad, M.;Rajesh Babu, B.;Ramesh, K.V.;Trinath, K.
    • Journal of Magnetics
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    • v.20 no.3
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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.

Diluted Synthesis of Manocrystalline CeO2 by Mechanical Milling (희석혼합체의 기계적 분쇄에 의한 나노 CeO2의 합성)

  • Lim, Geon-Ja;Kim, Tae-Eun;Lee, Jong-Ho;Lee, Hae-Weon;Rhee, Dong-Joo;Hyun, Sang-Hoon
    • Journal of the Korean Ceramic Society
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    • v.39 no.8
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    • pp.764-768
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    • 2002
  • The nanocrystalline $CeO_2$ was synthesized by mechanical milling and subsequent heat-treatment with the mixture of $Ce(OH)_4$ precursor and diluent, NaCl. Using deionized water, the diluent, NaCl, in the mixture has been easily dissolved out. Diffusion barrier was provided by the diluent during heat-treatment, which suppressed not only the coarsening of primary particle but also the agglormeration between the particles. Crystallite and aggregate size of $CeO_2$ depended on the concentration of diluent, temperature and time of heat-treatment; increased with the temperature and time increases. In case the mixture was heat-treated at high than $600^{\circ}C$, however, the crystallite size was saturated near 20 nm, which was supposed to be due to the densification of diluent.

Effect of M2O3 on the Sinterbility and Electrical Conductivity of ZrO2(Y2O3) System(III) : Ceramics of the ZrO2-Y2O3-Ln2O3 System (ZrO2(Y2O3)계 세라믹스의 소결성과 전기전도도에 대한 M2O3의 영향(III) : ZrO2-Y2O3-Ln2O3계 세라믹스)

  • 오영제;정형진;이희수
    • Journal of the Korean Ceramic Society
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    • v.24 no.2
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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.

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Characterization of Hexagonal Tungsten Bronze CsxWO3 Nanoparticles and Their Thin Films Prepared by Chemical Coprecipitation and Wet-Coating Methods

  • Kwak, Jun Young;Hwang, Tai Kyung;Jung, Young Hee;Park, Juyun;Kang, Yong-Cheol;Kim, Yeong Il
    • Journal of the Korean Chemical Society
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    • v.62 no.2
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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.