• Bulletin of the Korean Chemical Society
• /
• 제20권4호
• /
• pp.417-421
• /
• 1999

The complex, K3[La(TTHA)]5H,O, was prepared and its crystal structure was analyzed by single crystal X-ray diffraction method. In the complex, the La(Ⅲ) ion adopts a ten-coordinate geometry with four nitrogen atoms and six carboxyl oxygen atoms from the same TTHA ligand molecule. Its coordination polyhedron can be described as a distorted bicapped square antiprism. Each [La(TTHA)]3- anion is linked by K+ cations via carboxyl groups of TTHA ligand to form a three dimensional crystal structure. The thermal properties were investigated by TG and DTA techniques in argon atmosphere. The materials resulting from thermal treatment were La(OH)3 and K2O which were identified by powder X-ray diffraction technique.

• 한국분말재료학회지
• /
• 제14권5호
• /
• pp.309-314
• /
• 2007

Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using $ZrOCl_28H_2O$ and $NH_4OH$ under pH=11 and ambient condition. By this reaction. zirconia hydrate $(ZrO_x(OH)_{4-2x})$ was primarily synthesized and the obtained zirconia hydrate was heat treated hydrothermally using an autoclave at various temperatures under pH=11. X-ray diffraction, Scanning electron microscopy, Energy dispersive X-ray spectroscopy, FT-IR, Raman, Particle size analysis, DTA-TG, and BET techniques were used for the characterization of the powder. The synthesized zirconia showed an amorphous phase, however, the phase was transformed to the crystalline state during the hydrothermal process. The observed crystalline phase above $160^{\circ}C$ was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in $126{\sim}276m^2/g$ and the zirconia had the cylindrical shaped pores with average diameter of $2{\sim}7nm$.

• 한국대기환경학회지
• /
• 제26권1호
• /
• pp.1-9
• /
• 2010

In this study, the selective catalytic reduction of $NO_x$ with ammonia was carried out in a filter bag support reactor. The experiments were performed by powder type $MnO_x$ and $V_2O_5$/$TiO_2$ catalyst at low temperature between 130 and $250^{\circ}C$. Also, the effect of $SO_2$ and $H_2O$ on the NO conversion was investigated under our test conditions. The powder type catalysts were analyzed by X-ray photoelectron spectrum (XPS), X-ray diffraction(XRD), scanning electron microscopy (SEM) and thermal gravimetric analysis (TGA). It was observed that NO removal efficiency of the powder type $V_2O_5$/$TiO_2$ catalyst was 85% at low temperature($200^{\circ}C$) under presence of oxygen and that of $MnO_x$ was 50% at the same condition. The powder type $V_2O_5$/$TiO_2$ catalyst, in conclusion, was found to be available for SCR reaction in a filter bag support system.

• 한국잠사곤충학회지
• /
• 제37권2호
• /
• pp.142-153
• /
• 1995

특이한 분자 구조를 가진 생체 고분자로서 유용한 견 피브로인은 다양하게 성형 가공할 수 있으며 이를 위해서는 견 피브로인 수용액을 필요로 한다. 견 피브로인의 용해 조건이 형성되는 견 피브로인의 분말과 필름에 미치는 영향을 알아보기 위하여 종성염과 산가수분해법으로 견 피브로인을 용해시킨 수용액으로부터 견 피브로인 분말과 필름을 제조하고 이들의 특성을 아미노산 조정 분석, SEM, DSC, IR, X-ray Diffraction 등의 방법을 통하여 조사 분석한 결과는 다음과 같다. 1. 염화칼슘법과 염산법에 의해 피브로이을 용해시켰을 때 처리에 따라 아미노산 조성은 달랐으며 분자량도 차이가 있었다. 2. 분말의 구조 분석 결과, 염화칼슘법에 의한 처리에서 열분해 온도는 대조에 비해 낮게 나타났고 무정형의 분자 구조를 띄고 있음을 알 수 있었다. 염산 처리에 의한 잔유물은 대조보다 높은 온도에서 $\beta$구조에 의한 분해 거동을 보였으며 높은 결정화도를 나타냈다. 한편 염산에 용해된 부분은 열분해 분석 결과 a-helix에 의한 흡열 peak을 나타냈다. 3. 염화칼슘법에 의해 형성된 견 피브로인 필름은 모정형에 가까운 결정 구조를 가지고 있지만 불용화 처리에 의해 결정성이 향상됨에 따라 피브로인 필름의 흡습율은 감소하였으며, 열분해 온도가 증가했다.

• Bulletin of the Korean Chemical Society
• /
• 제5권4호
• /
• pp.135-140
• /
• 1984

The reduction of vacuum-dehydrated $Na_xAg_{12-x}-A, 0 {\le} x {\le} 9.2$, and its reoxidation by O$_2$, have been studied by X-ray powder diffraction. Also, the structure of $Na_6Na_6-A$ treated with hydrogen at room temperature has been studied by single crystal methods in the cubic space group Pm3m at $24{\circ}C (a = 12.221(2) {\AA})$. The diffraction pattern of dehydrated Ag$_{12}$-A reduced by H$_2$ contains only the (111) and (200) reflections of silver metal, indicationg that the zeolite structure has been lost, but the zeolite's diffraction pattern and structural integrity can be fully restored by oxidation with O$_2$ at 100 or 200${\circ}C$. In contrast, the structures of $Na_xAg_{12-x}-A$, x = 4.5 and 9.2, were not destroyed by treatment with hydrogen. Dehydrated Na$_6Ag_6$-A treated with 50 Torr of hydrogen gas at 24${\circ}C$ for 30 minutes has $6\; Na^+\;and\;1.27\;Ag^+$ ions at 6-ring sites. These $Ag^+ ions are associated with 2.54 Ag${\circ}$ atoms to form 1.27 $Ag_3^+$ clusters per unit cell. Also found were 0.7 $Ag_3^{2+}$ clusters per unit cell near the 8-rings. The structure was refined to the final error indices R$_1$ = 0.134 and R$_2$ (weighted) = 0.147, using 168 independent reflections for which $I_0 >3{\sigma}(I_0)$.

• 한국세라믹학회지
• /
• 제49권3호
• /
• pp.205-215
• /
• 2012

It has been studied the crystal and block structures of the hexagonal ferrites with M, W, Y and Z types prepared by various coprecipitation-oxidation method. The structures have been refined with a Rietveld analysis of the powder X-ray diffraction pattern with high precision ($R_{WP}$ <0.09, $R_I$ <0.03). The density difference between the S-blocks was proportioned to the cobalt contents in hexagonal ferrites, but that between the R or T-blocks was relatively small. Compared with the blocks and cation-oxygen polyhedra in BaM ($BaFe_{12}O_{19}$), those were bulky to the normal direction for the c-axis in $Co_2W$ ($BaCo_2Fe_{16}O_{27}$) and to the parallel direction for the c-axis in $Co_2Y$ ($Ba_2Co_2Fe_{12}O_{22}$) and $Co_2Z$ ($Ba_3Co_2Fe_{24}O_{41}$). The S-blocks of $Co_2W$, $Co_2Y$, and $Co_2Z$ were unstable and distorted. Because the T-block of $Co_2Z$ was unstable, the T-block was decomposed into the Ba-rich phase and $Co_2W$ at high temperatures above $1200^{\circ}C$. A standard powder X-ray diffraction pattern for $Co_2Z$ was proposed as well.

• Journal of Pharmaceutical Investigation
• /
• 제32권3호
• /
• pp.173-179
• /
• 2002

Solid dispersions of ipriflavone with PVP were prepared by a spray-drying method in order to improve the bioavailability. They were measured with scanning electron microscopy, differential scanning calorimetry, x-ray powder diffraction, and Fourier transform infrared spectroscopy to evaluate the physicochemical interaction between ipriflavone and PVP and study the correlation between these physicochemical characteristics and bioavailability. Ipriflavone exhibited crystallinity, whereas PVP was almost amorphous. The area of the endotherm $({\Delta}H)$ of freezer milled ipriflavone, freezer milled ipriflavone physically mixed with freezer milled PVP, and physically mixed ipriflavone with PVP was almost the same, whereas ${\Delta}H$ of the solid dispersed ipriflavone with PVP was much smaller than that of the other preparation types. Also, the crystallinity and the crystal size of ipriflavone in the solid dispersed ipriflavone with PVP were much smaller than those of the other preparation types. From the in vivo test, the AUC of the solid dispersed ipriflavone with PVP was approximately 10 times higher than that of the physically mixed ipriflavone with PVP. The solid dispersion using the spray-drying method with a water-soluble polymer, PVP, may be effective for the improvement of the bioavailability.

• 한국분말재료학회지
• /
• 제22권3호
• /
• pp.175-180
• /
• 2015

In this study, ternary compound Max Phase $Ti_2AlC$ material was mixed by 3D ball milling as a function of ball milling time. More than 99.5 wt% pure $Ti_2AlC$ was synthesized by using spark plasma sintering method at 1000, 1100, 1200, and $1300^{\circ}C$ for 60 min. The material characteristics of synthesized samples were examined with relative density, hardness, and electrical conductivity as a function of sintering temperature. The phase composition of bulk was identified by X-ray diffraction. On the basis of FE-SEM result, a terraced structures which consists of several laminated layers were observed. And $Ti_2AlC$ bulk material obtained a vickers hardness of 5.1 GPa at the sintering temperature of $1100^{\circ}C$.

• 한국결정학회지
• /
• 제14권2호
• /
• pp.79-83
• /
• 2003

Electrolytic MnO₂ (EMD)의 미세구조를 X선 회절 및 투과전자현미경 분석을 통해 연구하였다. 벌크에 대한 X선 회절 실험은 전헝적인 EMD 재료의 분말 회절패턴을 나타내었다. 투과전자현미경 분석은 EMD가 약 0.2㎛크기의 입자로 이루어져 있고, 각각의 입자가다시 10 nm 정도의 결정립으로 이루어진 이중 미세구조를 가짐을 나타내었다. 나노 결정립에 대한 전자빔 마이크로 회절 분석 결과, EMD 입자는 여러 상의 혼합체로서 약 50%의 Ramsdellite, 30%의 ε-MnO₂, 15%의 Pyrolusite 상으로 이루어져 있음을 확인하였다. 한편, X선 분말 회절패턴 상의 약 67°에 위치한 ｛1120｝ 피크와 (0001) 면에 대한 고분해능 이미지는 ε-MnO₂ 상의 존재를 입증하였다.

• 소성∙가공
• /
• 제26권4호
• /
• pp.216-221
• /
• 2017

Recently, interest in multifunctional energetic structural materials (MESMs) has grown due to their multifunctional potential, especially in military applications. However, there are few studies about extrinsic factors that govern the reactivity of MESMs. In this paper, a shock compaction process was performed on the nano Ni/Al-mixed powder to investigate the effect of particle size on the shock reaction condition. Additionally, heating the statically compacted specimen was also performed to compare the mechanical properties and microstructure between reacted and unreacted material. The results show that the agglomerated structure of nanopowders interrupts the reaction by reducing the elemental boundary. X-ray diffraction analysis shows that the NiAl and $Ni_3Al$ intermetallics are formed on the reacted specimen. The microhardness results show that the $Ni_3Al$ phase has a higher hardness than NiAl, but the portion of $Ni_3Al$ in the reacted specimen is minor. In conclusion, using Ni/Al composites as a reactive material should focus on energetic use.