• Title/Summary/Keyword: Amorphous powders

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X-ray Photoelectron Spectroscopy Study of LaFeO3 Powders Synthesized by Solution Combustion (용액연소법으로 제조한 LaFeO3의 XPS 특성)

  • Hwang, Yeon;Kang, Dae-Sik;Park, Mi-Hye;Cho, Sung-Baek
    • Korean Journal of Materials Research
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    • v.18 no.6
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    • pp.313-317
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    • 2008
  • [ $LaFeO_3$ ] powders were synthesized using a method involving solution combustion, and the surface properties of these powders were examined by x-ray photoelectron spectroscopy. As the amount of fuel increased during the synthesis, the $LaFeO_3$ powders became amorphous with a large plate-like shape. It was found that the O 1s spectra were composed of two types of photoelectrons by deconvolutioning the spectra. Photoelectrons with higher binding energy come from adsorbed oxygen ($O^-$) whereas those with lower energy come from lattice oxygen ($O^{2-}$). The ratio of adsorbed and lattice oxygen increased as the ratio of the fuel and nitrate (${\Phi}$) increased. The binding energy of both types of oxygen increased as ${\Phi}$ increased due to the formation of carbonates.

Synthesis and characterization of powders in the La-Al-Si-O system

  • Kyoung Jin Kim;Kwang Suk Joo;Kun Chul Shin;Keun Ho Auh;Kyo Seon Kim
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.5
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    • pp.475-479
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    • 1999
  • Langasite ($La_{3}Ga_{5}SiO_{14}$) was found to have wide application as a promising piezoelectric material. It has high thermal stability of the frequency and large electromechanical coupling factor. For the further development of new compounds with langasite type structure, powders in the La-Al-Si-O system were synthesized by a modified Pechini process. The evolution of the crystalline phase during calcination was studied using TG-DTA, XRD and TEM for the precursor powders. Decomposition proceeded via dehydration and removal of excess solvents at low temperatures ($T<500^{\circ}C$), followed by the crystallization of lanthanum aluminum silicate ($T>800^{\circ}C$) and phase transformation to $LaAlO_{3}$ phase ($T>1200^{\circ}C$). Transmission electron microscopy (TEM) of the calcined powders showed diffuse hollow rings corresponding to an amorphous phase at $800^{\circ}C$ and clear diffraction patterns corresponding to a crystalline phase from the P321 space group ($T<1200^{\circ}C$) and the R3m ($T<1200^{\circ}C$).

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The Preparation of Blue CoAl2O4 Powders by the Malonate Method: The Effect of the Amount of Malonic Acid Used, the Formation Pathway of CoAl2O4 Crystallites and the Characteristics of the Prepared Powders

  • Lee, Gong-Yeol;Ryu, Kwang-Hyun;Kim, Hong-Gun;Kim, Yoo-Young
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.373-377
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    • 2009
  • A pathway for the formation of normal $CoAl_2O_4$ particles is suggested. The optimal amount of malonic acid was determined, and the characteristics of the obtained powders were investigated. Normal $CoAl_2O_4$ powders were prepared using solutions of malonic acid and metal nitrates. X-ray diffraction, Brunauer-Emmett-Teller (BET) and scanning electron microscope (SEM) measurements, as well as Fourier transform infrared (FTIR) and ultraviolet/visible (UV-Vis) spectroscopy were carried out. Normal $CoAl_2O_4$ crystallites were formed by a solid state reaction between $CoAl_2O_4$ and amorphous aluminum oxide. The optimal molar ratio of malonic acid to the nitrate anions present in the initial solution was found to be 0.30~0.35. The particles were composed of agglomerates of primary particles. The primary particles were 40 nm in size. This size was relatively constant regardless of the preparation temperature. However, the size of the agglomerated particles increased to 220 nm with increasing temperature.

Phase Analysis of Immiscible V-Cu MA Powders by Neutron and X-ray Diffraction (비고용 V-Cu계 MA합금의 중성자 및 X선 회절에 의한 상분석)

  • Lee Chung-Hyo;Cho Jae-Moon;Lee Sang-Jin;Kim Ji-Soon
    • Korean Journal of Materials Research
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    • v.14 no.5
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    • pp.348-352
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    • 2004
  • The mechanical alloying (MA) effect in immiscible V-Cu system with positive heat of mixing was studied by not only the neutron and X-ray diffraction but also the analysis of DSC spectra. The total energy, ΔHt accumulated during MA for the mixture of $V_{50}$ $Cu_{50}$ / powders increased with milling time and approached the saturation value of 14 kJ/mol after 120 h of milling. It can be seen that the free energy difference between the amorphous phase and the pure V and Cu powders with an atomic ratio 5:5 is estimated to be 11 kJ/mol by Miedema et al. This is thermodynamically taken as one of the evidences for the amorphization. The structural changes of V-Cu MA powders were characterized by the X-ray diffraction and neutron diffraction. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. The neutron diffraction data definitely indicate that the amorphization proceeds gradually but incompletely even after 120 h of MA and bcc-Cu Bragg peaks appears after 60 h of MA.

Preparation of Ga2O3:Eu3+ Phosphor by Pechini Method (Pechini법에 의한 Ga2O3:Eu3+ 형광체 분말의 제조)

  • Park, In-Yong;Lee, Jong-Won;Kim, Seon-Tai
    • Korean Journal of Materials Research
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    • v.12 no.7
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    • pp.517-521
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    • 2002
  • Europium-activated $Ga_2$$O_3$ phosphor powders were prepared by Pechini method from the mixed aqueous solutions of gallium(III) nitrate, europium(III) nitrate, ethylene glycol and citric acid. The phase formation process and particle shape of the powders obtained were investigated by means of TG/DTA, XRD and SEM. It was found that the powders were amorphous or ${\gamma}$-$Ga_2$$O_3$-like phase up to $500^{\circ}C$ and then transformed into $\beta$- $Ga_2$$O_3$ phase above $600 ^{\circ}C$. The powders calcined below $1000^{\circ}C$ were spherical and nanometer-sized. Photoluminescence spectra measured at room temperature showed that the highest luminescence intensity was obtained for the sample synthesized under the conditions of 2 mol% Eu concentration and heat treatment at $1000^{\circ}C$.

Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders (기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화)

  • 이충효;전성용;김지순
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.4
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    • pp.129-134
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    • 2004
  • In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

Synthesis of amorphous Fe-Cr-N alloy powders by mechanical alloying (기계적 합금화에 의한 Fe-Cr-N 계 비정질 합금분말의 제조)

  • 이충효
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.1
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    • pp.132-136
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    • 1999
  • Mechanical alloying (MA) by ball mill of $Fe_{30}Cr_{70}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed in this case, while MA under an inert argon gas atmosphere produces the bcc solid solution. The DSC spectrum for the mechanically alloyed $(Fe_{30}Cr_{70})_{0.85}N_{0.15)$powders exhibits a sharp exothermic peak due to crystallization at about $550^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was observed through X-ray and neutron diffractions. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is situated at a center of the tetrahedron formed by metal atoms.

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The Formation and Crystallization of Amorphous Ti50Cu50Ni20Al10 Powder Prepared by High-Energy Ball Milling

  • Viet, Nguyen Hoang;Kim, Jin-Chun;Kim, Ji-Soon;Kwon, Young-Soon
    • Journal of Powder Materials
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    • v.16 no.1
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    • pp.9-15
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    • 2009
  • Amorphization and crystallization behaviors of $Ti_{50}Cu_{50}Ni_{20}Al_{10}$ powders during high-energy ball milling and subsequent heat treatment were studied. Full amorphization obtained after milling for 30 h was confirmed by X-ray diffraction and transmission electron microscope. The morphology of powders prepared using different milling times was observed by field-emission scanning electron microscope. The powders developed a fine, layered, homogeneous structure with prolonged milling. The crystallization behavior showed that the glass transition, $T_g$, onset crystallization, $T_x$, and super cooled liquid range ${\Delta}T=T_x-T_g$ were 691,771 and 80 K, respectively. The isothermal transformation kinetics was analyzed by the John-Mehn-Avrami equation. The Avrami exponent was close to 2.5, which corresponds to the transformation process with a diffusion-controlled type at nearly constant nucleation rate. The activation energy of crystallization for the alloy in the isothermal annealing process calculated using an Arrhenius plot was 345 kJ/mol.

Synthesis of TiN/TiB2/Ti-silicides Nanocomposite Powders by Mechanochemical Reaction and its Reaction Mechanism (기계화학반응에 의한 TiN/TiB2/Ti-silicides 나노복합분말의 합성과 반응기구)

  • Cho Young-Whan;Kim Ji-Woo;Shim Jae-Hyeok;Ahn Jae-Pyoung;Oh Kyu-Hwan
    • Journal of Powder Materials
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    • v.12 no.4 s.51
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    • pp.273-278
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    • 2005
  • Nanostructured TiN/$TiB_2$/$TiSi_2$ and TiN/$TiB_2$/$Ti_5Si_2$ composite powders have been prepared by mechanochemical reaction from mixtures of Ti, BN, and $Si_3N_4$ powders. The raw materials have reacted to form a uniform mixture of TiN, $TiB_2$ and $TiSi_2$ or $Ti_5Si_3$ depending on the amount of $Si_3N_4$ used in the starting mixtures, and the reaction proceeded through so-called mechanically activated self-sustaining reaction (MSR). Fine TiN and $TiB_2$ crystallites less than a few tens of nanometer were homogeneously dispersed in the amorphous $TiSi_2$ or $Ti_5Si_3$ matrix after milling for 12 hours. These amorphous matrices became crystalline phases after annealing at high temperatures as expected, but the original microstructure did not change significantly.

Effect of Powder Preheating Temperature on the Properties of Cu based Amorphous Coatings by Cold Spray Deposition (저온분사로 제조된 Cu계 비정질 코팅층 특성에 미치는 분말 예열 온도의 영향)

  • Cho, Jin-Hyeon;Park, Dong-Yong;Lee, Jin-Kyu;Lee, Kee-Ahn
    • Korean Journal of Metals and Materials
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    • v.47 no.11
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    • pp.728-733
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    • 2009
  • Cu based amorphous ($Cu_{54}Zr_{22}Ti_{18}Ni_{6}$) powders were deposited onto Al 6061 substrates by cold spray process with different powder preheating temperatures (below glass transition temperature: $350^{\circ}C$, near glass transition temperature: $430^{\circ}C$ and near crystallization temperature: $500^{\circ}C$). The microstructure and macroscopic properties (hardness, wear and corrosion) of Cu based amorphous coating layers were also investigated. X-ray diffraction results showed that cold sprayed Cu based amorphous coating layers of $300{\sim}350{\mu}m$ thickness could be well manufactured regardless of powder preheating temperature. Porosity measurements revealed that the coating layers of $430^{\circ}C$ and $500^{\circ}C$ preheating temperature conditions had lower porosity contents (0.88%, 0.93%) than that of the $350^{\circ}C$ preheating condition (4.87%). Hardness was measured as 374.8 Hv ($350^{\circ}C$), 436.3 Hv ($430^{\circ}C$) and 455.4 Hv ($500^{\circ}C$) for the Cu based amorphous coating layers, respectively. The results of the suga test for the wear resistance property also corresponded well to the hardness results. The critical anodic current density ($i_{c}$) according to powder preheating temperature conditions of $430^{\circ}C$, $500^{\circ}C$ was lower than that of the sample preheated at $350^{\circ}C$, respectively. The higher hardness, wear and corrosion resistances of the preheating conditions of near $T_{g}$ and $T_{x}$, compared to the properties of below $T_{g}$, could be well explained by the lower porosity of coating layer.