• Title/Summary/Keyword: low temperature scanning electron microscopy

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Mechanical Strength Evaluation of A53B Carbon Steel Subjected to High Temperature Hydrogen Attack

  • Kim, Maan-Won;Lee, Joon-Won;Yoon, Kee-Bong;Park, Jai-Hak
    • International Journal of Safety
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    • v.6 no.2
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    • pp.1-7
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    • 2007
  • In this study mechanical strength of A53B carbon steel was analyzed using several types of test specimens directly machined from oil recycling pipe experienced a failure due to hydrogen attack in chemical plants. High temperature hydrogen attack (HTHA) is the damage process of grain boundary facets due to a chemical reaction of carbides with hydrogen, thus forming cavities with high pressure methane gas. Driven by the methane gas pressure, the cavities grow on grain boundaries forming intergranular micro cracks. Microscopic optical examination, tensile test, Charpy impact test, hardness measurement, and small punch (SP) test were performed. Carbon content of the hydrogen attacked specimens was dramatically reduced compared with that of standard specification of A53B. Traces of decarburization and micro-cracks were observed by optical and scanning electron microscopy. Charpy impact energy in hydrogen attacked part of the pipe exhibited very low values due to the decarburization and micro fissure formation by HTHA, on the other hand, data tested from the sound part of the pipe showed high and scattered impact energy. Maximum reaction forces and ductility in SP test were decreased at hydrogen attacked part of the pipe compared with sound part of the pipe. Finite element analyses for SP test were performed to estimate tensile properties for untested part of the pipe in tensile test. And fracture toughness was calculated using an equivalent strain concept with SP test and finite element analysis results.

The behaviour of strength and fatigue crack propagation of various steels in steel bridges (철강구조물 부재의 강도평가 및 피로균열진전거동)

  • Han, Seung-Ho;Kim, Jung-Kyu
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.21 no.10
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    • pp.1694-1701
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    • 1997
  • The residual safety assessment of steel structures, an important subject in practice, is given to much attention. Life prediction in the planning course of steel structures under fatigue loading is mainly based on fatigue design criteria resulting from S-N curves. But for any reason cracks have to be assumed due to fabrication failures or fatigue loading in service which can lead total fracture of structures. The life prediction can be carried out by means of fracture mechanics using Paris-Erdogan equation($da/dN=C {\cdot}{\Delta}K^m$). The paper presents results from charpy test to interpret transition behaviour of charpy energy($A_V$) in a wide temperature range and from constant-load-amplitude test to measure fatigue crack growth of various steels widely used in steel bridges since beginning of 20 centuries in Europe. In the normal service temperature range of steel bridges, the steel S355M shows higher maximum charpy energy($A_{Vmax}$) and lower transition temperature($T_{AVmax/2}$) than other steels considered. The C and m of Paris-Erdogan equation on the steels appear to be correlated, and to be affected by the R-ratios due to crack closure, especially at a low fatigue crack growth rate. Scanning electron microscopy analysis was carried out to interpret an influence of the crack closure effects on the correlation of C and m.

Physicochemical and Gelatinization Properties of Glutinous Rice Flour and Starch Steeped at Different Conditions (수침한 찹쌀가루와 전분의 이화학적 및 호화 특성)

  • 최은정;김향숙
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.26 no.1
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    • pp.17-24
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    • 1997
  • The effects of steeping on the physicochemical and gelatinization characteristics of glutinous rice flour and its starch were studied. Steeping conditions were 1 day at 25"C,7 days at 2iC and 7 days at 35"C. Crude protein, lipid and ash content were decreased br steeping. It was observed with scanning electron microscopy that endosperm cell wall of glutinous rice flour was diminished by steeping. Although morphology of the glutinous rice starch granules was not affected, the size was decreased by steeping. Density and water binding capacity(WBC) of glutinous rice flour and its starch were changed by steeping. X-ray diffraction pattern of glutinous rice starch was A type and was not affected by steeping. Swelling power of glutinous rice flour and its starch was increased but solubility was decreased by steeping. In Brabender amylographic examination, peak viscosity of untreated glutinous rice flour was very low and increased enormously by steeping resulting in the similar Brabender viscosity pattern to its starch. The gelatinization temperature examined by X-ray diffractometry was lowered by steeping. And the degree of gelatinization under the conclusion temperature increased with increasing of steeping Period and temperature.mperature.

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Synthesis and Characterization of NiAl2O4 Inorganic Pigment Nanoparticles by a Reverse Micelle Processing (역-마이셀 공정에 의한 NiAl2O4 무기안료 나노 분말의 합성 및 특성)

  • Son, Jeong-Hun;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.25 no.2
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    • pp.95-99
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    • 2015
  • $NiAl_2O_4$ nanoparticle was synthesized by a reverse micelle processing for inorganic pigment. $Ni(NO_3)_2{\cdot}6H_2O$ and $Al(NO_3)_3{\cdot}9H_2O$ were used for the precursor in order to synthesize $NiAl_2O_4$ nanoparticles. The aqueous solution, which consisted of a mixing molar ratio of Ni/Al, was 1:2 and heat treated at $800{\sim}1100^{\circ}C$ for 2h. The average size and distribution of synthesized $NiAl_2O_4$ powders are in the range of 10-20 nm and narrow, respectively. The average size of the synthesized $NiAl_2O_4$ powders increased with an increasing water-to-surfactant molar ratio and heating temperature. The crystallinity of synthesized $NiAl_2O_4$ powder increased with an increasing heating temperature. The synthesized $NiAl_2O_4$ powders were characterized by X-ray diffraction analysis(XRD), a field emission scanning electron microscopy(FE-SEM), and a color spectrophotometer. The properties of synthesized powders were affected as a function such as a molar ratio and heating temperature. Results indicate that synthesis using a reverse miclle processing is a favorable process to obtain $NiAl_2O_4$ spinels at low temperatures. The procedure performed suggests that this new synthesis route for producing these oxides has the advantage of being fast and simple. Colorimetric coordinates indicate that the pigments obtained exhibit blue colors.

Effect of the Substrate Temperature on the Characteristics of CIGS Thin Films by RF Magnetron Sputtering Using a $Cu(In_{1-x}Ga_x)Se_2$ Single Target

  • Jung, Sung-Hee;Kong, Seon-Mi;Fan, Rong;Chung, Chee-Won
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.382-382
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    • 2012
  • CIGS thin films have received great attention as a promising material for solar cells due to their high absorption coefficient, appropriate bandgap, long-term stability, and low cost production. CIGS thin films are deposited by various methods such as co-evaporation, sputtering, spray pyrolysis and electro-deposition. The deposition technique is one of the most important processes in preparing CIGS thin film solar cells. Among these methods, co-evaporation is one of the best technique for obtaining high quality and stoichiometric CIGS films. However, co-evaporation method is known to be unsuitable for commercialization. The sputtering is known to be very effective and feasible process for mass production. In this study, CIGS thin films have prepared by rf magnetron sputtering using a $Cu(In_{1-x}Ga_x)Se_2$ single quaternary target without post deposition selenization. This process has been examined by the effects of deposition parameters on the structural and compositional properties of the films. In addition, we will explore the influences of substrate temperature and additional annealing treatment after deposition on the characteristics of CIGS thin films. The thickness of CIGS films will be measured by Tencor-P1 profiler. The crystalline properties and surface morphology of the films will be analyzed using X-ray diffraction and scanning electron microscopy, respectively. The optical properties of the films will be determined by UV-Visible spectroscopy. Electrical properties of the films will be measured using van der Pauw geometry and Hall effect measurement at room temperature using indium ohmic contacts.

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Effect of CuO-V2O5 Addition on Microwave Dielectric Properties of (Pb0.45Ca0.55(Fe0.5Nb0.5)0.9Sn0.1]O3 Ceramics

  • Ha, Jong-Yoon;Choi, Ji-Won;Yoon, Ki-Hyun;Choi, Doo-Jin;Yoon, Seok-Jin;Kim, Hyun-Jai
    • Journal of the Korean Ceramic Society
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    • v.41 no.1
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    • pp.9-12
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    • 2004
  • The effect of x wt% CuO-y wt% $V_2O_5$ content on the microwave properties of $(Pb_{0.45}Ca_{0.55})[(Fe_{0.5}Nb_{0.5})_{0.9}Sn_{0.1}]O_3$ (PCFNS) ceramics was investigated. In order to decrease the sintering temperature and use as a Low Temperature co-firing Ceramics (LTCC), CuO-$V_2O_5$ are added in the PCFNS. The bulk density, dielectric constant (${\varepsilon}_r$) and quality factor(Q${\cdot}f_0$) increased with increase in CuO content within a limited value. The microwave properties were degraded with increases in $V_2O_5$ content. The temperature coefficient of the resonant frequency (${\tau}_f$) of PCFNS was shifted to positive value abruptly with increasing the $V_2O_5$ content, while the ${\tau}_f$ was slightly shifted to positive value with increasing the CuO content. The optimized microwave properties, ${\varepsilon}_r$ = 88, Q${\cdot}f_0$ = 6100 (GHz), and ${\tau}_f$ = 18 ppm/$^{\circ}C$, were obtained in $(Pb_{0.45}Ca_{0.55})[(Fe_{0.5}Nb_{0.5})_{0.9}Sn_{0.1}]O_3$ with 0.2wt% CuO 0.05 wt% $V_2O_5$ and sintered at $1000^{\circ}C$ for 3 h. The relationship between the microstructure and microwave dielectric properties of ceramics was studied by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM)

Dielectric properties of SBT($SrBi_2Ta_2O_9$) on $Bi_2O_3$/Pt/Ti/$SiO_2$/Si substrate accordiing to various substrate temperature of $Bi_2O_3$ buffer layer (Si(100)기판에 $SrBi_2Ta_2O_9$ 박막증착 시 $Bi_2O_3$ 후열처리에 따른 유전특성)

  • Yoon, Ji-Eon;Cha, Won-Hyo;Lee, Chul-Su;Son, Young-Guk
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.200-201
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    • 2007
  • The SBT($SrBi_2Ta_2O_9$) thin films with $Bi_2O_3$ buffer layer were deposited on Pt/Ti/$SiO_2$/Si substrate by R.F. magnetron sputtering method in order to improve the ferroelectric characteristics. In SBT thin films, the deficiency of bismuth during the process due to its volatility results in an obvious non stoichiometry of the films and the presence of secondary phases. $Bi_2O_3$ buffer layer was found to be effective to achieve the low temperature crystallization and improve the ferroelectric properties of SBT thin films. Ferroelectric properties and crystallinities of SBT thin films with various post annealing of $Bi_2O_3$ buffer layer were observed as various annealing temperature, using X-Ray Diffraction (XRD), scanning electron microscopy (SEM), Keithley 237 and HP 4192A Impedance Analyzer.

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Thermal Compression of Copper-to-Copper Direct Bonding by Copper films Electrodeposited at Low Temperature and High Current Density (저온 및 고전류밀도 조건에서 전기도금된 구리 박막 간의 열-압착 직접 접합)

  • Lee, Chae-Rin;Lee, Jin-Hyeon;Park, Gi-Mun;Yu, Bong-Yeong
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.102-102
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    • 2018
  • Electronic industry had required the finer size and the higher performance of the device. Therefore, 3-D die stacking technology such as TSV (through silicon via) and micro-bump had been used. Moreover, by the development of the 3-D die stacking technology, 3-D structure such as chip to chip (c2c) and chip to wafer (c2w) had become practicable. These technologies led to the appearance of HBM (high bandwidth memory). HBM was type of the memory, which is composed of several stacked layers of the memory chips. Each memory chips were connected by TSV and micro-bump. Thus, HBM had lower RC delay and higher performance of data processing than the conventional memory. Moreover, due to the development of the IT industry such as, AI (artificial intelligence), IOT (internet of things), and VR (virtual reality), the lower pitch size and the higher density were required to micro-electronics. Particularly, to obtain the fine pitch, some of the method such as copper pillar, nickel diffusion barrier, and tin-silver or tin-silver-copper based bump had been utillized. TCB (thermal compression bonding) and reflow process (thermal aging) were conventional method to bond between tin-silver or tin-silver-copper caps in the temperature range of 200 to 300 degrees. However, because of tin overflow which caused by higher operating temperature than melting point of Tin ($232^{\circ}C$), there would be the danger of bump bridge failure in fine-pitch bonding. Furthermore, regulating the phase of IMC (intermetallic compound) which was located between nickel diffusion barrier and bump, had a lot of problems. For example, an excess of kirkendall void which provides site of brittle fracture occurs at IMC layer after reflow process. The essential solution to reduce the difficulty of bump bonding process is copper to copper direct bonding below $300^{\circ}C$. In this study, in order to improve the problem of bump bonding process, copper to copper direct bonding was performed below $300^{\circ}C$. The driving force of bonding was the self-annealing properties of electrodeposited Cu with high defect density. The self-annealing property originated in high defect density and non-equilibrium grain boundaries at the triple junction. The electrodeposited Cu at high current density and low bath temperature was fabricated by electroplating on copper deposited silicon wafer. The copper-copper bonding experiments was conducted using thermal pressing machine. The condition of investigation such as thermal parameter and pressure parameter were varied to acquire proper bonded specimens. The bonded interface was characterized by SEM (scanning electron microscope) and OM (optical microscope). The density of grain boundary and defects were examined by TEM (transmission electron microscopy).

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Silicide Formation of Atomic Layer Deposition Co Using Ti and Ru Capping Layer

  • Yoon, Jae-Hong;Lee, Han-Bo-Ram;Gu, Gil-Ho;Park, Chan-Gyung;Kim, Hyung-Jun
    • Korean Journal of Materials Research
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    • v.22 no.4
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    • pp.202-206
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    • 2012
  • $CoSi_2$ was formed through annealing of atomic layer deposition Co thin films. Co ALD was carried out using bis(N,N'-diisopropylacetamidinato) cobalt ($Co(iPr-AMD)_2$) as a precursor and $NH_3$ as a reactant; this reaction produced a highly conformal Co film with low resistivity ($50\;{\mu}{\Omega}cm$). To prevent oxygen contamination, $ex-situ$ sputtered Ti and $in-situ$ ALD Ru were used as capping layers, and the silicide formation prepared by rapid thermal annealing (RTA) was used for comparison. Ru ALD was carried out with (Dimethylcyclopendienyl)(Ethylcyclopentadienyl) Ruthenium ((DMPD)(EtCp)Ru) and $O_2$ as a precursor and reactant, respectively; the resulting material has good conformality of as much as 90% in structure of high aspect ratio. X-ray diffraction showed that $CoSi_2$ was in a poly-crystalline state and formed at over $800^{\circ}C$ of annealing temperature for both cases. To investigate the as-deposited and annealed sample with each capping layer, high resolution scanning transmission electron microscopy (STEM) was employed with electron energy loss spectroscopy (EELS). After annealing, in the case of the Ti capping layer, $CoSi_2$ about 40 nm thick was formed while the $SiO_x$ interlayer, which is the native oxide, became thinner due to oxygen scavenging property of Ti. Although Si diffusion toward the outside occurred in the Ru capping layer case, and the Ru layer was not as good as the sputtered Ti layer, in terms of the lack of scavenging oxygen, the Ru layer prepared by the ALD process, with high conformality, acted as a capping layer, resulting in the prevention of oxidation and the formation of $CoSi_2$.

Synthesis of rhombohedral-structured zinc germanate thin films and characteristics of divalent manganese-activated electroluminescence

  • Yoon, Kyung-Ho;Kim, Joo-Han
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.453-453
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    • 2010
  • In this study, zinc germanate ($Zn_2GeO_4$) thin films has been synthesized by using radio frequency magnetron sputtering and the divalent manganese-activated luminescence was characterized. X-ray diffraction patterns of the as-deposited $Zn_2GeO_4$:Mn films showed only a broad feature, indicative of an amorphous structure. Scanning electron microscopy images revealed that the as-deposited $Zn_2GeO_4$:Mn has a smooth surface morphology. The $Zn_2GeO_4$:Mn films were found to be crystallized by annealing in air ambient at temperatures as low as $700^{\circ}C$. The annealed $Zn_2GeO_4$:Mn possessed a rhombohedral polycrystalline structure. The broad-band photoluminescent emission spectrum from 470 to 650nm was obtained at room temperature from the $Zn_2GeO_4$:Mn films. The emission peak was centered at around 535nm in the green range, which originates from the intrashell transition of manganese $3d^5$ electrons from $^4T_1$ excited-state level to the $^6A_1$ ground state. The PL emission spectrum had an asymmetric line shape, which results from the $^3d_5$ electron transitions of divalent manganese ions located at different sites of the zinc germanate host crystal lattice. Electroluminescent devices were fabricated using $Zn_2GeO_4$:Mn as an emission layer. The fabricated devices showed a green EL emission similar to the PL emission. The CIE chromaticity color coordinates of the EL emission were determined to be x=0.308 and y=0.657.

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