Synthesis of ZnCo2O3 oxide is performed by sol-gel method via nitrate-citrate route. Powder X-ray diffraction (XRD) study shows monoclinic unit cell having lattice parameters: a = 5.721(1) Å, b = 8.073(2) Å, c = 5.670(1) Å, β = 93.221(8)°, space group P2/m and Z = 4. Average crystallite sizes determined by Scherrer equation are the range ~14-32 nm, whereas SEM micrographs show nano-micro meter size particles formed in ZnCo2O3. Endothermic peak at ~798 K in the Differential scanning calorimetric (DSC) trace without weight loss could be due to structural transformation and the endothermic peak ~1143 K with weight loss is due to reversible loss of O2 in air atmosphere. Energy Dispersive X-ray (EDX) analysis profile shows the presence of elements Zn, Co and O which indicates the purity of the sample. Magnetic measurements in the range of +12 kOe to -12 kOe at 10 K, 77 K, 120 K and at 300 K by PPMS-II Physical Property Measurement System (PPMS) shows hysteresis loops having very low values of the coercivity and retentivity which indicates the weakly ferromagnetic nature of the oxide. Observed X-band EPR isotropic lineshapes at 300 K and 77 K show positive g-shift at giso ~2.230 and giso ~2.217, respectively which is in agreement with the presence of paramagnetic site Co2+(3d7) in the oxide. DC conductivity value of 2.875 ×10-8 S/cm indicates very weakly semiconducting nature of ZnCo2O3 at 300 K. DRS absorption bands ~357 nm, ~572 nm, ~619 nm and ~654 nm are due to the d-d transitions 4T1g(4F)→2Eg(2G), 4T1g(4F)→4T1g(4P), 4T1g(4F)→4A2g(4F), 4T1g(4F)→4T2g(4F), respectively in octahedral ligand field around Co2+ ions. Direct band gap energy, Eg~ 1.5 eV in the oxide is obtained by extrapolating the linear part of the Tauc plot to the energy axis indicates fairly strong semiconducting nature of ZnCo2O3.
Passive fitting of meso-structure and super-structures is a predominant requirement for the longevity and clinical success of osseointegrated dental implants. However, precision and passive fitting has been unpredictable with conventional methods of casting as well as for corrective techniques. Alternative to conventional techniques, electro discharge machining(EDM) is an advanced method introduced to dental technology to improve the passive fitting of implant prosthesis. In this technique material is removed by melting and vaporization in electric sparks. Regarding the efficacy of EDM, the application of this technique induces severe surface morphological and elemental alterations due to the high temperatures developed during machining, which vary between $10,000{\sim}20,000^{\circ}C$. The aim of this study was to investigate the morphological and elemental alterations induced by EDM process of casting dental gold alloy and non-precious alloy used for the production of implant-supported prosthesis. A conventional clinical dental casting alloys were used for experimental specimens patterns, which were divided in three groups, high fineness gold alloy(Au 75%, HG group), low fineness gold alloy(Au 55%, LG group) and nonprecious metal alloy(Ni-Cr, NP group). The UCLA type plastic abutment patterns were invested with conventional investment material and were cast in a centrifugal casting machine. Castings were sandblasted with $50{\mu}m\;Al_2O_3$. One casting specimen of each group was polished by conventional finishing(HGCON, LGCON, NPCON) and one specimen of each group was subjected to EDM in a system using Cu electrodes, kerosene as dielectric fluid in 10 min for gold alloy and 20 min for Ni-Cr alloy(HGEDM. LGEDM, NOEDM). The surface morphology of all specimens was studied under an energy dispersive X-ray spectrometer (EDS). The quantitative results from EDS analysis are presented on the HGEDM and LGEDM specimens a significant increase in C and Cu concentrations was found after EDM finishing. The different result was documented for C on the NPEDM with a significant uptake of O after EDM finishing, whereas Al, Si showed a significant decrease in their concentrations. EDS analysis showed a serious uptake of C and Cu after the EDM procedure in the alloys studied. The C uptake after the EDM process is a common finding and it is attributed to the decomposition of the dielectric fluid in the plasma column, probably due to the development of extremely high temperatures. The Cu uptake is readily explained from the decomposition of Cu electrodes, something which is also a common finding after the EDM procedure. However, all the aforementioned mechanisms require further research. The clinical implication of these findings is related with the biological and corrosion resistance of surfaces prepared by the EDM process.
Ti-50 at. % Ni 합금 타깃으로 PLD(pulsed laser deposition)방법을 사용하여 TiNi 형상기억합금 박막을 제작하였다. Ar분위기(200 mTorr)와 고진공분위기($5{\times}10^{-6}\;Torr$)에서 제작한 TiNi 박막의 조성 및 결정성의 변화를 조사했으며, 박막의 조성은 에너지 분산 엑스선 분광 분석(EDXS)을 이용하여 조사하였고, 박막의 결정성은 엑스선 회절장치(XRD)를 이용하여 조사하였다. 박막의 조성은 기판과 타깃의 거리에 의존되었지만, 기판의 온도와는 무관함을 알 수 있었으며, Ar 분위기에서 플룸 안쪽에 기판이 위치하였을 때 조성 제어가 용이함을 알 수 있었다. 또한, Ar 가스 분위기에서 증착 된 TiNi 박막은 고진공분위기에서 증착된 박막보다 더 낮은 온도(약 $400^{\circ}C$)에서 in situ로 결정화됨을 알 수 있었다. 이들 결과는, PLD방법으로 TiNi 형상기억합금 박막을 제작할 때 분위기 가스의 압력이 결정화 온도를 낮추어 주는 중요한 역할을 할 수 있음을 시사한다.
This document was prepared to review and summarize the analytical methods for airborne and bulk asbestos. Basic principles, shortcomings and advantages for asbestos analytical instruments using phase contrast microscopy(PCM), polarized light microscopy(PLM), X-ray diffractometer (XRD), transmission electron microscopy(TEM), scanning electron microscopy(SEM) were reviewed. Both PCM and PLM are principal instrument for airborne and bulk asbestos analysis, respectively. If needed, analytical electron microscopy is employed to confirm asbestos identification. PCM is used originally for workplace airborne asbestos fiber and its application has been expanded to measure airborne fiber. Shortcoming of PCM is that it cannot differentiate true asbestos from non asbestos fiber form and its low resolution limit ($0.2{\sim}0.25{\mu}m$). The measurement of airborne asbestos fiber can be performed by EPA's Asbestos Hazard Emergency Response Act (AHERA) method, World Health Organization (WHO) method, International Standard Organization (ISO) 10312 method, Japan's Environmental Asbestos Monitoring method, and Standard method of Indoor Air Quality of Korea. The measurement of airborne asbestos fiber in workplace can be performed by National Institute for Occupational Safety and Health (NIOSH) 7400 method, NIOSH 7402 method, Occupational Safety and Health Administration (OSHA) ID-160 method, UK's Health and Safety Executive(HSE) Methods for the determination of hazardous substances (MDHS) 39/4 method and Korea Occupational Safety and Health Agency (KOSHA) CODE-A-1-2004 method of Korea. To analyze the bulk asbestos, stereo microscope (SM) and PLM is required by EPA -600/R-93/116 method. Most bulk asbestos can be identified by SM and PLM but one limitation of PLM is that it can not see very thin fiber (i.e., < $0.25{\mu}m$). Bulk asbestos analytical methods, including EPA-600/M4-82-020, EPA-600/R-93/116, OSHA ID-191, Laboratory approval program of New York were reviewed. Also, analytical methods for asbestos in soil, dust, water were briefly discussed. Analytical electron microscope, a transmission electron microscope equipped with selected area electron diffraction (SAED) and energy dispersive X-ray analyser(EDXA), has been known to be better to identify asbestiform than scanning electron microscope(SEM). Though there is no standard SEM procedures, SEM is known to be more suitable to analyze long, thin fiber and more cost-effective. Field emission scanning electron microscope (FE-SEM) imaging protocol was developed to identify asbestos fiber. Although many asbestos analytical methods are available, there is no method that can be applied to all type of samples. In order to detect asbestos with confidence, all advantages and disadvantages of each instrument and method for given sample should be considered.
Microstructural changes during tempering at the temperature range of $300^{\circ}C{\sim}700^{\circ}C$ for the nitrogen-permeated STS 410 and 410L martensitic stainless steels has been investigated. After nitrogen permeation at temperature between 1050 and $1150^{\circ}C$, the surface layer appeared fine $Cr_2N$ of square and rod types in the martensite matrices. Hardness of the nitrogen-permeated surface layer represented 680Hv and 625Hv, respectively, for 410 and 410L steels. It is considered that the fine homogeneously dispersive effect of precipitates by nitrogen caused the increased hardness. Due to the counter current effect of carbon from interior to surface during nitrogen diffusion from surface to interior, the 0.1%C alloyed 410 steel showed the low nitrogen content of 0.025% compared with 0.045% of 410L steel at the distance of $100{\mu}m$ from the surface. Tempering of nitrogen-alloyed 410 and 410L showed the maximum hardness at $450^{\circ}C$. This maximum hardness was considered to be the secondary hardening effect of very fine carbide and nitride. The decrease in hardness at $700^{\circ}C$ was the softening effect of the matrix due to the precipitation of many needle-shaped $Cr_2N$ for 410 steel and the precipitation of coarse nitride of $Cr_2N$ in line with the spherical precipitates with directionality for 410L steel. For 410 steel, the corrosion resistance of nitrogen permeated surface in the solution of 1 N $H_2SO_4$ were nearly unchanged, however the superior corrosion resistance was obtained for nitrogen permeated 410L steel compared to the solution annealed condition.
Sn-Bi eutectic alloy has been widely used as one of the key solder materials for step soldering at low temperature. The Sn-58Bi solder paste containing chloride flux was adopted to compare with that using the chloride-free flux. The paste was applied on the electroless nickel-immersion gold (ENIG) surface finish by stencil printing, and the reflow process was then performed at $170^{\circ}C$ for 10 min. After reflow, the solder joints were aged at $125^{\circ}C$ for 100, 200, 300, 500 and 1000 h in an oven. The interfacial microstructures were obtained by using scanning electron microscopy (SEM), and the composition of intermetallic compounds (IMCs) was analyzed using energy dispersive spectrometer (EDS). Two different IMC layers, consisting of $Ni_3Sn_4$ and relatively very thin Sn-Bi-Ni-Au were formed at the solder/surface finish interface, and their thickness increased with increasing aging time. The wettability of solder joints was investigated by wetting balance test. The mechanical property of each aging solder joint was evaluated by the ball shear test in accordance with JEDEC standard (JESD22-B117A). The results show that the highest shear force was measured when the aging time was 100 h, and the fracture mode changed from ductile fracture to brittle fracture with increasing aging time. On the other hand, the chloride flux in the solder paste did not affect the shear force and fracture mode of the solder joints.
Objectives: 3D printing technologies have become widely developed and are increasingly being used for a variety of purposes. Recently, the evaluation of 3D printing operations has been conducted through chamber test studies, and actual workplace studies have yet to be completed. Therefore, the objective of this study was to determine the emission of volatile organic compounds(VOCs), metals, and particles from printing operations at a workplace. This included monitoring conducted at a commercial 3D printing service workplace where the processes involved material extrusion, material jetting, binder jetting, vat photo polymerization, and powder bed fusion. Methods: Area samples were collected with using a Tenax TA tube for VOC emission and MCE filter for metals in the workplace. For particle monitoring, Mini Particle Samplers(MPS) were also placed in the printer, indoor work area, and outdoor area. The objective was to analyze and identify particles' size, morphology, and chemical composition using transmission electron microscopy with energy dispersive spectroscopy(TEM-EDS) in the workplace. Results: The monitoring revealed that the concentration of VOCs and metals generated during the 3D printing process was low. However, it also revealed that within the 3D printing area, the highest concentration of total volatile organic compounds(TVOC) was 4,164 ppb at the vat photopolymerization 3D printing workplace, and the lowest was 148 ppb at the material extrusion 3D printing workplace. For the metals monitoring, chromium, which, is carcinogenic for humans, was detected in the workplace. As a characteristic of the particles, nano-sized particles were also found during the monitoring, but most of them were agglomerated with large and small particles. Conclusions: Based on the monitoring conducted at the commercial 3D printing operation, the results revealed that the concentration of VOCs and metals in the workplace were within Korea's occupational exposure limits. However, due to the emission of nano-sized particles during 3D printing operations, it was recommended that the exposure to VOCs and metals in the workplace should be minimized out of concern for workers' health. It was also shown that the characteristics of particles emitted from 3D printing operations may spread widely within an indoor workplace.
We report the structural characterization of $Bi_xZn_{1-x}O$ thin films grown on c-plane sapphire substrates by plasma-assisted molecular beam epitaxy. By increasing the Bi flux during the growth process, $Bi_xZn_{1-x}O$ thin films with various Bi contents (x = 0~13.17 atomic %) were prepared. X-ray diffraction (XRD) measurements revealed the formation of Bi-oxide phase in (Bi)ZnO after increasing the Bi content. However, it was impossible to determine whether the formed Bi-oxide phase was the monoclinic structure ${\alpha}-Bi_2O_3$ or the tetragonal structure ${\beta}-Bi_2O_3$ by means of XRD ${\theta}-2{\theta}$ measurements, as the observed diffraction peaks of the $2{\theta}$ value at ~28 were very close to reflection of the (012) plane for the monoclinic structure ${\alpha}-Bi_2O_3$ at 28.064 and the reflection of the (201) plane for the tetragonal structure ${\beta}-Bi_2O_3$ at 27.946. By means of transmission electron microscopy (TEM) using a diffraction pattern analysis and a high-resolution lattice image, it was finally determined as the monoclinic structure ${\alpha}-Bi_2O_3$ phase. To investigate the distribution of the Bi and Bi-oxide phases in BiZnO films, elemental mapping using energy dispersive spectroscopy equipped with TEM was performed. Considering both the XRD and the elemental mapping results, it was concluded that hexagonal-structure wurtzite $Bi_xZn_{1-x}O$ thin films were grown at a low Bi content (x = ~2.37 atomic %) without the formation of ${\alpha}-Bi_2O_3$. However, the increased Bi content (x = 4.63~13.17 atomic %) resulted in the formation of the ${\alpha}-Bi_2O_3$ phase in the wurtzite (Bi)ZnO matrix.
Jung, Yoonhee;Lim, Jong-Myoung;Ji, Young-Yong;Chung, Kun Ho;Kang, Mun Ja
Journal of Radiation Protection and Research
/
제42권1호
/
pp.33-41
/
2017
Background: Phosphate rock and its by-product are widely used in various industries to produce phosphoric acid, gypsum, gypsum board, and fertilizer. Owing to its high level of natural radioactive nuclides (e.g., $^{238}U$ and $^{226}Ra$), the radiological safety of workers who work with phosphate rock should be systematically managed. In this study, $^{238}U$, $^{232}Th$, $^{226}Ra$, and $^{40}K$ levels were measured to analyze the transport characteristics of these radionuclides in the production cycle of phosphate rock. Materials and Methods: Energy dispersive X-ray fluorescence and gamma spectrometry were used to determine the activity of $^{238}U$, $^{232}Th$, $^{226}Ra$, and $^{40}K$. To evaluate the extent of secular disequilibrium, the analytical results were compared using statistical methods. Finally, the distribution of radioactivity across different stages of the phosphate rock production cycle was evaluated. Results and Discussion: The concentration ratios of $^{226}Ra$ and $^{238}U$ in phosphate rock were close to 1.0, while those found in gypsum and fertilizer were extremely different, reflecting disequilibrium after the chemical reaction process. The nuclide with the highest activity level in the production cycle of phosphate rock was $^{40}K$, and the median $^{40}K$ activity was $8.972Bq{\cdot}g^{-1}$ and $1.496Bq{\cdot}g^{-1}$, respectively. For the $^{238}U$ series, the activity of $^{238}U$ and $^{226}Ra$ was greatest in phosphate rock, and the distribution of activity values clearly showed the transport characteristics of the radionuclides, both for the byproducts of the decay sequences and for their final products. Conclusion: Although the activity of $^{40}K$ in k-related fertilizer was relatively high, it made a relatively low contribution to the total radiological effect. However, the activity levels of $^{226}Ra$ and $^{238}U$ in phosphate rock were found to be relatively high, near the upper end of the acceptable limits. Therefore, it is necessary to systematically manage the radiological safety of workers engaged in phosphate rock processing.
Crystallographic characteristics and interfacial structures of $Al_2$$O_3$and $ZrO_2$dielectric films prepared by atomic layer chemical vapor deposition (ALCVD) were investigated at atomic scale by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDS)/electron energy-loss spectroscopy (EELS) coupled with a field-emission transmission electron microscope. The results obtained from cross-sectional and plan-view specimens showed that the $Al_2$$O_3$film was crystallized by annealing at a high temperature and its crystal system might be evaluated as either cubic or tetragonal phase. Whereas the $ZrO_2$film crystallized during deposition at a low temperature of ∼$300^{\circ}C$ was composed of both tetragonal and monoclinic phase. The interfacial thickness in both films was increased with the increased annealing temperature. Further, the interfacial structures of X$ZrO_2$$O_3$and $ZrO_2$films were discussed through analyses of EDS elemental maps and EELS spectra obtained from the annealed films, respectively.
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