• 대한화학회지
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• 제68권2호
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• pp.82-86
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• 2024

This paper presents the solid-state synthesis of insoluble Prussian blue (Fe₄[Fe(CN)₆]₃·xH₂O, PB) in a ball mill, utilizing the fundamental components of PB. Solid-state synthesis offers several advantages, such as being solvent-free, quantitative, and easily scalable for industrial production. Traditionally, the solid-state synthesis of PB has been limited to the reaction between iron(II/III) ions and hexacyanoferrate(II/III) complex ions, essentially an extension of the solution-based coprecipitation method to solid-state reaction. Taking a bottom-up approach, a reaction is designed where the reactants consist of the basic building blocks of PB: Fe²⁺ ions and CN^- ions. The reaction, with a molar ratio of Fe²⁺ and CN^- corresponding to 1:2.8, yields PB, while a ratio of 1:6.6 results in a mixture of potassium hexacyanoferrate(II) (K₄Fe(CN)₆), potassium chloride (KCl), and potassium cyanide (KCN). This synthetic approach holds promise for environmentally friendly methods to synthesize multimetallic PB with maximum entropy in nearly quantitative yield.

• 한국신재생에너지학회:학술대회논문집
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• 한국신재생에너지학회 2009년도 춘계학술대회 논문집
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• pp.134-137
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• 2009

Commercially available elemental powders of Cu, Zn, Sn and Se were employed for crystallizing a stannite-type $Cu_2ZnSnSe_4$ compound by means of solid state reaction. $Cu_2ZnSnSe_4$ reaction chemistry was also modeled based on differential-thermal analysis and X-ray powder diffraction results. It was observed that Se tends to react preferably with Cu to form CuSe and $CuSe_2$ phases at low reaction temperature. The formation of $Cu_5Zn_8$ intermetallic phase was found to be the intermediate reaction path for the binary ZnSe formation. A solid state reaction at $320^{\circ}C$ reacted elemental powderst obinary selenides of CuSe, ZnSe and SnSe completely. The crystallization of $Cu_2ZnSnSe_4$ was was detected to begin at $300^{\circ}C$ and its weight fraction increased with an increase of reaction temperature, which most probably formed from the reaction between $Cu_2SnSe_3$ and ZnSe.

• 한국세라믹학회지
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• 제37권5호
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• pp.459-465
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• 2000

3CaO.3Al2O3.CaSO4(C4A3)clinker was prepared by solid state reaction and then its hydration property was investigated. C4A3 clinker was fired at various temperatures in the range of 700~135$0^{\circ}C$. The hydration of it was studied by XRD, DSC, Solid-state 27Al MAS NMR and SEM. According to the results, the Ca4A3 clinker was produced by reacting calcium aluminates with CaSO4 and Al2O3 and C4A3 was formed as a main phase after calcining at 120$0^{\circ}C$. The hydration products were mainly calcium monosulfoaluminate hydrate and Al(OH)3, and they were produced after 2hrs of hydration. However the hydration rate was about 74% at 3days.

• 한국세라믹학회지
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• 제54권3호
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• pp.217-221
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• 2017

Improvement studies of existing phosphors are needed for use in light emitting diodes (LEDs). Among the phosphors discovered recently, the SLA ($SrLiAl_3N_4:Eu^{2+}$) is a phosphor that has a narrow width. It is now known as a good red phosphor that meets the industry's needs for warm white (color temperature ranging from 2700 to 4000 K) and high CRI (> 80). However, SLA phosphors are obtained from difficult synthetic methods. All commercially available phosphors should be derived from the general solid state synthesis method. The phosphors produced by difficult synthetic methods will inevitably fall out of price competitiveness and will be scrapped. This study succeeded in synthesizing SLA ($SrLiAl_3N_4:Eu^{2+}$) phosphors by using a general solid phase synthesis method based on the reaction energy obtained from DFT calculations. As a result, we found an optimal solid state synthesis method for SLA phosphors.

• Journal of Magnetics
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• 제19권1호
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• pp.64-67
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• 2014

$Ni_{0.6}Zn_{0.4}Fe_2O_4$ prepared using solid state reaction and sol-gel methods were compared for their structural and magnetic properties. Due to the much higher annealing temperature used in solid state reaction, the crystalline size was much larger than that of the nanoparticles prepared by sol-gel. The saturation magnetization of sol-gel nanoparticles was higher, and the coercivity was about 2 times larger, compared to the solid state reaction sample. By analyzing the integration intensity of x-ray diffraction peaks (220) and (222), we proposed that the difference in the saturation magnetization might be due to the inversion of cation distribution caused by the different preparation techniques used.

• 한국재료학회지
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• 제15권7호
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• pp.473-479
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• 2005

Thermoelectric $Zn_4Sb_3$ alloys were synthesized by a conventional powder metallurgy process consisting of solid state reaction and hot pressing. Single phase $Zn_4Sb_3$ was successfully produced by the annealing of cold compact starting with the mixed elemental powders, and subsequent hot pressing yielded single phase bulk specimens without microcracks. Phase transformations in this alloy system during synthesis were investigated using XRD, SEM and EDS. Thermoelectric properties as a function of temperature were investigated from room temperature to 600 K and compared with results of analogue studies. Transport properties at room temperature were also evaluated. Thermoelectric properties of single phase $Zn_4Sb_3$ materials produced by this process are comparable to the published data. Synthesis by solid state reaction and hot pressing offers a potential processing route to produce a bulk $Zn_4Sb_3$.ٓ

• 한국재료학회지
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• 제34권6호
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• pp.309-314
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• 2024

The structure and magnetic properties of composite powders prepared by ball milling a mixture of Fe₂O₃·(0.4-1.0)Fe were investigated. Hysteresis loops and differential scanning calorimetry (DSC) curves are used to characterize the materials and to examine the effect of the solid state reaction induced by ball milling. The results showed that a solid state reaction in Fe₂O₃·(0.4-1.0)Fe clearly proceeds after only 1 h of ball milling. The system is characterized by a positive reaction heat of +2.23 kcal/mole. The diffraction lines related to Fe₂O₃ and Fe disappeared after 1 h of ball milling and, instead, diffraction lines of the intermediate phase of Fe₃O₄ plus FeO formed. The magnetization and coercivity of the Fe₂O₃·0.8Fe powders were changed by the solid state reaction process of Fe₂O₃ by Fe during ball milling. The coercivity of the Fe₂O₃·0.8Fe powders increased with increasing milling time and reached a maximum value of 340 Oe after 5 h of ball milling. This indicates the grain size of Fe₃O₄ was clearly reduced during ball milling. The magnetic properties of the annealed powders depend on the amount of magnetic Fe and Fe₃O₄ phases.

• 한국세라믹학회지
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• 제19권2호
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• pp.109-114
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• 1982

Fluoro-phlogopite crystals (Mica) were synthesized by two different methods; firstly the crystal was crystallized from the melts, and secondly mica crystalline was obtained from the direct solid state reaction. Addition of $CaF_2$ in the mica batch revealed the lowering the solid state reaction temperature. SEM and XRD were employed to observe mica crystalline flakes and solid solution forms. As a starting raw material Pyrophyllite was used resulting in the formation of mica crystals.

• E2M - 전기 전자와 첨단 소재
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• 제10권2호
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• pp.141-149
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• 1997

L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders were prepared by both GNP(Glycine-Nitrate Process) and solid state reaction method in various of calcination temperature(800-1000.deg. C) and time in air. Also, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contacts on YSZ(Yttria-Stabilized Zirconia) substrate were prepared by screen printing and sintering method as a function of sintering temperature(1100-1450.deg. C) in air. Sintering behaviors have been investigated by SEM(Scanning Electron Microscope) and porosity measurement. Compositional and structural characterization were carried out by X-ray diffractometer and ICP AES(Inductively Coupled Plasma-Atomic Emission Spectrometry) analysis. Electrical characterization was carried out by the electrical conductivity with linear 4 point probe method. As the calcination period increased in solid state reaction method, L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ phase increased. Although L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ single phase was obtained only for 48hrs at 1000.deg. C, in GNP method it was easy to get single and ultra-fine L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ powders with submicron particle size at 650.deg. C for 30min. The particle size and thickness of L $a_{0.7}$S $r_{0.3}$Mn $O_{3}$ cathode contact by solid state reaction method did not change during the heat treatment, while those by GNP method showed good sintering characteristics because initial powder size fabricated from GNP method is smaller than that fabricated from solid state reaction method. Based on enthalpy change from thermodynamic data and ICP-AES analysis, it was suggested to make cathode contact in composition of (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$ Mn $O_{3}$ which have little second phase (L $a_{2}$Z $r_{2}$ $O_{7}$) for high efficient solid oxide fuel cells applications. As (L $a_{0.7}$S $r_{0.3}$)$_{0.91}$Mn $O_{3}$ cathode contact on YSZ substrate was sintering at 1250.deg. C the temperature that liquid phase sintering did not occur. It was possible to obtain proper cathode contacts with electrical conductivity of 150(S/cm) and porosity content of 30-40%.m) and porosity content of 30-40%.

• Journal of Mechanical Science and Technology
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• 제15권4호
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• pp.473-481
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• 2001

By depicting the transfer of heat and combustion reaction to take place within thin gas layers close to the propellant surface burning in a steady-state fashion, a mathematical equation has been deduced to describe the burning rate of solid propellant as a function of initial grain temperature and chamber pressure. It has been also assumed that chemical reaction could take place in premixing-diffusing zone but were carried out mainly in the reaction-flame zone. All these phenomena taken place in each zone of combustion have been assumed to be steady-state. In the present investigation, the equation, γ=$\kappa$$.$(1/R(T(sub)i+C))(sup)n$.$exp(-E(sub)a/R(T(sub)i+C))(P/z) is being presented and it is compared with experimental data. The proposed model has been tested and evaluated vis-a-vis strand burner data for three different propellants based on CTPB, and it has been found that the deviation of the computed burning rates from the measured rates ranged up to 2%.