• Title/Summary/Keyword: X-ray Diffractometer

Search Result 601, Processing Time 0.022 seconds

Chain extension effects of para-phenylene diisocyanate on crystallization behavior and biodegradability of poly(lactic acid)/poly(butylene terephthalate) blends (파라-페닐렌 다이이소시아네이트의 사슬 연장이 PLA/PBT 블렌드의 결정화 거동과 생분해성에 미치는 영향)

  • Kim, Myung-Wook;Hong, Sung-Min;Lee, Doo-Jin;Park, Kwang-Seok;Youn, Jae-Ryoun
    • Composites Research
    • /
    • v.22 no.3
    • /
    • pp.18-28
    • /
    • 2009
  • Blends of poly(lactic acid) (PLA) and poly(butylene terephthalate) (PBT) were prepared by reaction extrusion with para-phenylene diisocyanate (PPDI). The crystallization behavior and biodegradability were investigated by using a differential scanning calorimeter (DSC), a wide angle X-ray diffractometer (WAXD), a contact angle goniometer, and a buffer solution containing esterase. The addition of PBT into PLA polymer matrix induced the cold crystallization of PLA phase, and the crystallization rate of PLA phase was significantly accelerated when both PBT and PPDI participated in the reaction with PLA simultaneously. But the chain extension caused by PPDI decreased the crystallinity and hydrophilicity of PLA and PBT phases. The crystallinity and hydrophilicity did not affect the biodegradability of PLA/PBT blends. However, phase separation between PLA and PBT in PLA/PBT blends increased the interfacial area exposed to the hydrolysis of enzyme, resulting in the improved degradability rate of PLA phase. In contrast, the improved interfacial adhesion between PLA and PBT matrices by the reaction with PPDI reduced the area exposed to the enzyme to decrease the degradation rate of PLA phase.

Sol-gel synthesis, computational chemistry, and applications of Cao nanoparticles for the remediation of methyl orange contaminated water

  • Nnabuk Okon Eddy;Rajni Garg;Rishav Garg;Samson I. Eze;Emeka Chima Ogoko;Henrietta Ijeoma Kelle;Richard Alexis Ukpe;Raphael Ogbodo;Favour Chijoke
    • Advances in nano research
    • /
    • v.15 no.1
    • /
    • pp.35-48
    • /
    • 2023
  • Nanoparticles are known for their outstanding properties such as particle size, surface area, optical and electrical properties. These properties have significantly boasted their applications in various surface phenomena. In this work, calcium oxide nanoparticles were synthesized from periwinkle shells as an approach towards waste management through resource recovery. The sol gel method was used for the synthesis. The nanoparticles were characterized using X-Ray diffractometer (XRD), Fourier Transformed Infra-Red Spectrophotometer (FTIR), Brunauer Emmett Teller (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultra violet visible spectrophotometer (UV-visible). While DLS and SEM underestimate the particle diameter, the BET analysis reveals surface area of 138.998 m2/g, pore volume = 0.167 m3/g and pore diameter of 2.47 nm. The nanoparticles were also employed as an adsorbent for the purification of dye (methyl orange) contaminated water. The adsorbent showed excellent removal efficiency (up to 97 %) for the dye through the mechanism of physical adsorption. The adsorption of the dye fitted the Langmuir and Temkin models. Analysis of FTIR spectrum after adsorption complemented with computational chemistry modelling to reveal the imine nitrogen group as the site for the adsorption of the dye unto the nanomaterials. The synthesized nanomaterials have an average particle size of 24 nm, showed a unique XRD peak and is thermally and mechanically stable within the investigated temperature range (30 to 70 ℃).

Study on the Geochemical Weathering Process of Sandstones and Mudstones in Pohang Basin at CO2 Storage Condition (지중저장 조건에서 초임계CO2에 의한 포항분지 사암과 이암의 지화학적 풍화반응 연구)

  • Park, Jinyoung;Lee, Minhee;Wang, Sookyun
    • Economic and Environmental Geology
    • /
    • v.46 no.3
    • /
    • pp.221-234
    • /
    • 2013
  • Laboratory experiments for the reaction with supercritical $CO_2$ under the $CO_2$ sequestration condition were performed to investigate the mineralogical and geochemical weathering process of the sandstones and mudstones in the Pohang basin. To simulate the supercritical $CO_2$-rock-groundwater reaction, rock samples used in the experiment were pulverized and the high pressurized cell (200 ml of capacity) was filled with 100 ml of groundwater and 30 g of powdered rock samples. The void space of the high pressurized cell was saturated with the supercritical $CO_2$ and maintained at 100 bar and $50^{\circ}C$ for 60 days. The changes of mineralogical and geochemical properties of rocks were measured by using XRD (X-Ray Diffractometer) and BET (Brunauer-Emmett-Teller). Concentrations of dissolved cations in groundwater were also measured for 60 days of the supercritical $CO_2$-rock-groundwater reaction. Results of XRD analyses indicated that the proportion of plagioclase and K-feldspar in the sandstone decreased and the proportion of illite, pyrite and smectite increased during the reaction. In the case of mudstone, the proportion of illite and kaolinite and cabonate-fluorapatite increased during the reaction. Concentration of $Ca^{2+}$ and $Na^+$ dissolved in groundwater increased during the reaction, suggesting that calcite and feldspars of the sandstone and mudstone would be significantly dissolved when it contacts with supercritical $CO_2$ and groundwater at $CO_2$ sequestration sites in Pohang basin. The average specific surface area of sandstone and mudstone using BET analysis increased from $27.3m^2/g$ and $19.6m^2/g$ to $28.6m^2/g$ and $26.6m^2/g$, respectively, and the average size of micro scale void spaces for the sandstone and mudstone decreased over 60 days reaction, resulting in the increase of micro pore spaces of rocks by the dissolution. Results suggested that the injection of supercritical $CO_2$ in Pohang basin would affect the physical property change of rocks and also $CO_2$ storage capacity in Pohang basin.

Removal of Fluoride Using Thermally Treated Activated Alumina (고온 처리된 활성알루미나를 이용한 불소 제거)

  • Park, Seong-Jik;Kim, Jae-Hyeon;Lee, Chang-Gu;Park, Jeong-Ann;Choi, Nag-Choul;Kim, Song-Bae
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.32 no.10
    • /
    • pp.986-993
    • /
    • 2010
  • In this study, sorption characteristics of thermally treated activated alumina (AA) for fluoride were investigated. Sorption experiments have been conducted in equilibrium and kinetic batch conditions. Also, effects of solution pH and anions on fluoride removal have been observed. The properties of thermally treated ( $700^{\circ}C$) activated alumina (AA700) and untreated activated alumina (UAA) were compared using field-emission scanning electron microscope, energy-dispersive spectrometry, X-ray diffractometer (XRD) analysis, and Brunauer-Emmett-Teller (BET) analysis. From the experiments using AA thermally treated at different temperatures (100, 300, 500, $700^{\circ}C$), it was found that at high fluoride concentrations (50, 100, 200 mg/L) the sorption capacity of thermally treated AA increased with increasing thermal treatment temperature. At an initial fluoride concentration of 200 mg/L, the sorption capacity of AA700 was 3.67 times greater than that of UAA. The BET analysis showed that the specific surface area of UAA was about 2 times larger than that of AA700. The XRD analysis indicated that UAA was composed of both boehmite (AlOOH) and bayerite ($Al(OH)_3$) while AA700 was $Al_2O_3$. The reason that fluoride sorption capacity of AA700 increased despite of decrease in specific surface area compared to UAA could be attributed to the change of crystal structure. The kinetic sorption test showed that fluoride sorption to AA700 arrived at equilibrium after 24 h. The equilibrium test demonstrated that the maximum sorption capacity of AA700 was 5.70 mg/g. Additional batch experiments indicated that fluoride sorption to AA700 was the highest at pH 7, decreasing at both acidic and basic solution pHs. Also, fluoride sorption to AA700 decreased in the presence of anions such as phosphate, nitrate, and carbonate. This study demonstrated that thermal treatment of AA at high temperature could increase its sorption capacity for fluoride.

Effects of acid-treatment conditions on the surface properties of the RBM treated titanium implants (산-처리 조건이 RBM처리한 티타늄 임플란트의 표면 특성에 주는 영향)

  • Lee, Han-Ah;Seok, Soohwang;Lee, Sang-Hyeok;Lim, Bum-Soon
    • Korean Journal of Dental Materials
    • /
    • v.45 no.4
    • /
    • pp.257-274
    • /
    • 2018
  • The purpose of this study was to evaluate the effect of acid-treatment conditions on the surface properties of the RBM (Resorbable Blast Media) treated titanium. Disk typed cp-titanium specimens were prepared and RBM treatments was performed with calcium phosphate ceramic powder. Acid solution was mixed using HCl, $H_2SO_4$ and deionized water with 4 different volume fraction. The RBM treated titanium was acid treated with different acid solutions at 3 different temperatures and for 3 different periods. After acid-treatments, samples were cleaned with 1 % Solujet solution for 30 min and deionized water for 30 min using ultrasonic cleanser, then dried in the electrical oven ($37^{\circ}C$). Weight of samples before and after acid-treatment were measured using electric balance. Surface roughness was estimated using a confocal laser scanning microscopy, crystal phase in the surface of sample was analyzed using X-ray diffractometer. Surface morphology and components were evaluated using Scanning Electron Microscope (SEM) with Energy Dispersive X-ray spectroscopy (EDX) and X-ray Photoemission Spectroscopy (XPS). Values of the weight changes and surface roughness were statistically analyzed using Tukey-multiple comparison test (p=0.05). Weight change after acid treatments were significantly increased with increasing the concentration of $H_2SO_4$ and temperature of acid-solution. Acid-treatment conditions (concentration of $H_2SO_4$, temperature and time) did not produce consistent effects on the surface roughness, it showed the scattered results. From XRD analysis, formation of titanium hydrides in the titanium surface were observed in all specimens treated with acid-solutions. From XPS analysis, thin titanium oxide layer in the acid-treated specimens could be evaluated. Acid solution with $90^{\circ}C$ showed the strong effect on the titanium surface, it should be treated with caution to avoid the over-etching process.

The Crystal Structure of Bis(N-Methylphenazinium) Bis(Oxalato)Palladate(Ⅱ) (Bis(N-Methylphenazinium) Bis(Oxalato)Palladate(Ⅱ)의 결정구조)

  • Kim, Se Hwan;NamGung, Hae;Lee, Hyeon Mi
    • Journal of the Korean Chemical Society
    • /
    • v.38 no.11
    • /
    • pp.827-832
    • /
    • 1994
  • The crystal structure of bis(N-methylphenazinium) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: ((C_{13}H_{11}N_2)_2[Pd(C_2O_4)_2]) $M_w$ = 672.93, Triclinic, Space Group P1 (No = 2), a = 7.616(8), b = 9.842(3), c = $20.335(7)\AA$, $\alpha$ = 103.53(3), $\beta$ = 90.00(5), $\gamma$ = $112.38(5)^{\circ}$, Z = 2, $V = 1363(2){\AA}^3\;D_c = 1.639\;gcm^{-3},\;{\mu} = 7.3\;cm^{-1},\;F(000) = 680.0$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$= 0.7107\;\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-square methods using Killean & Lawrence weights. The final R and S values were $R = 0.069,\;R_w = 0.050,\;R_{all} = 0.069$ and S = 5.45 for 3120 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angles of 6.3(6) and $57.06(6)^{\circ}$ between their planes. The planar complex anions are sandwiched between slightly bent cations. The interplanar separations of two triads are 3.328 and 3.463 $\AA$, respectively. The triads are stacked along b-axis, but their orientations are different based on dihedral angle $59.08(9)^{\circ}$ of two complex anions.

  • PDF

Bone Cements in TTCP, DCPA, β-TCP and PHA System (TTCP-DCPA-β-TCP-PHA계 골 시멘트)

  • ;;;Rainer Telle
    • Journal of the Korean Ceramic Society
    • /
    • v.39 no.1
    • /
    • pp.57-67
    • /
    • 2002
  • The effect of $\beta$-TCP and PHA as additives on initial setting time, compressive strength and surface micro-structure after in vitro test of bone cement in TTCP and DCPA system was investigated. The median particle sizes of TTCP, $\beta$-TCP, DCPA and PHA for bone cement were about 3, 5, 0.9 and 4${\mu}{\textrm}{m}$, respectively. Initial setting time and compressive strength of bone cement with various composition was measured by Vicat test and Universal Testing Machine, and surface morphology and crystalline phases of bone cements were observed and analyzed by SEM and x-ray diffractometer. Initial setting time was not affected by composition but by powder/liquid ratio, and cement with PHA required double amount of solution for paste as much as one without PHA, especially. It was thought that $\beta$-TCP and PHA in bone cements was not related to setting reaction. Thus, the addition of $\beta$-TCP and PHA in bone cements decreased compressive strength and inhabited HAP from being produced on surface in vitro test. In conclusion, it was not expected that $\beta$-TCP and PHA in TTCP-DCPD bone cements enhanced the strength and bioacitivity.

The Crystal Structure of Bis(1,2-diaminopropane)palladium(Ⅱ) Bis(oxalato)palladate(Ⅱ) (Bis(1,2-diaminopropane)palladium(Ⅱ) Bis(oxalato)palladate(Ⅱ)의 결정구조)

  • Kim Sei Hwan;NagGung Hae;Jeon, Ho Jung
    • Journal of the Korean Chemical Society
    • /
    • v.37 no.6
    • /
    • pp.599-603
    • /
    • 1993
  • Crystal structure of bis(1,2-diaminopropane)palladium(II) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: $Pd_2C_{10}H_{10}N_{4}O_{8}$, $M_W$ = 573.09, orthorhombic, space group $P_{ccn}$ (No = 56), a = 16.178(5), b = 16.381(6), c = 6.685(2)$\{AA}$, V = 1771.6 $\{AA}^3$, $M_W$W = 573.09, $D_c$ = 2.014 g${\cdot}c\;m^{-3}$, Z = 4, T = 294K, F(000) = 1056.0 and $\mu$ = 20.466 c$m^{-1}$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$ = 0.7107 $\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-squares methods using Pivot weights. The final R and S values were R = 0.065, $R_W = 0.059, R_{all}$ = 0.065 and S = 4.315 for 605 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angle of $18(l)^{\circ}$ between thier planes. In the crystal structure, they do not have the Magnus's salt type mixed stacks; instead, the complex anions form regular stacks along the c-axis with the M-M bond length of $3.343(5)\AA$ and their stacks are surrounded by the complex cations through hydrogen bonds with the nitrogen-oxygen distances of 2.94(3) and $3.31(4)\AA.$

  • PDF

The Crystal Structure of Tris(ethylenediamine)nickel(II)-dichromate, $[Ni(C_2N_2H_8)_3]\cdotCr_2O_7$ ($[Ni(C_2N_2H_8)_3]\cdotCr_2O_7$의 결정구조)

  • Kim, Se-Hwan;Kim, Seung-Bin;Nam, Gung-Hae
    • Korean Journal of Crystallography
    • /
    • v.7 no.1
    • /
    • pp.36-43
    • /
    • 1996
  • The crystal structure Tris(ethylenediamine)nickel(II)Dichromate has been determined by X-ray crystallography. Crystal data: a=8.268(2), b=13.865(2), c=14.921(2)Å, γ=102.04(2)°, V=1672.9(5)Å3, Z=4, Monocline, P21/b (space group No.=14), Dcalc=1.806 gcm-3, μ=24.05 cm-0.1. The intensity data were collected with Mo-Kα radiation(λ=0.7107Å) on an automatic four-circle diffractometer with a graphite monochromator. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.045, Rw=0.051, Rall=0.059 and S=2.171for 2248 observed reflections. The two carbon atoms of a ring of Ni(en)-ion were split into crossed four atoms. In consideration of α- and β-angles of two rings of a disordered ethylenediamine of Nien3-ion and the hydrogen bonds between Ni(en)3-cation and Cr2O7-anion, the configuration of Ni(en)3-ion is assumed to be disordered with Λδδδ and Λδδλ.

  • PDF

Mossbauer Studies of the $H_2$ Reduction Effects On Magnetic Properties of Sr-Ba Substituted Hexgonal Ferrite (치환형 Sr-Ba 육방 페라이트들의 자기적 성질에 수소환원이 미치는 효과에 관한 Mossbauer 분광학적 연구)

  • 박재윤;권명회;이재광
    • Journal of the Korean Magnetics Society
    • /
    • v.9 no.1
    • /
    • pp.35-40
    • /
    • 1999
  • Sr substituted materials for some barium in M-type barium ferrite powder and Co-Ti substituted Sr-Ba hexagonal ferrite powder were prepared by citrate sol-gel method and 2 MOE sol-gel method these hexaferrite particles were reduced for 1hr in the hydrogen gas. The reduction temperatures were varied in the range of 250 $^{\circ}C$ to 500 $^{\circ}C$. X-ray diffraction patterns were measured using diffractometer with Cu $K_{\Alhpa}$ radiation. Mossbauer absorption spectra were measured with a constant acceleration spectrometer. We have focused on studying the origin of increasing $M_s$ by M$\"{o}$ssbauer spectroscopy. Ferrite particles which were sintered at 105$0^{\circ}C$ were found to be typical magnetoplumbite structure and single phase. XRD patterns with varying the reduction temperatures in $Sr_{0.5}Ba_{0.5}Fe_{10}O_{19}$ indicates ferrites particles become composite hexaferrites containing $\alpha$-Fe at T_{red}=350 \;$^{\circ}C$$. On the otherhand, it was found that $Co^{2+}$ ions and $Ti^{4+}$ ions in $Sr_{0.7}Ba_{0.3}Fe_{10}CoTiO_{19}$ prevent from changing $Fe^{3+}$ ions to $\alpha$-Fe during the $H_2$ reduction. Comparing Mossbauer results with XRD results, we have determined most of $\alpha$-Fe are reduced from $4f_{vi}$ sites and 12k sites of $Fe^{3+}$ ions. These $\alpha$-Fe phase bring the induced anisotropy and increase saturation magnetization $M_s$.TEX>.

  • PDF