• Title/Summary/Keyword: High-temperature XRD

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Formation Mechanisms of Sn Oxide Films on Probe Pins Contacted with Pb-Free Solder Bumps (무연솔더 범프 접촉 탐침 핀의 Sn 산화막 형성 기제)

  • Bae, Kyoo-Sik
    • Korean Journal of Materials Research
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    • v.22 no.10
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    • pp.545-551
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    • 2012
  • In semiconductor manufacturing, the circuit integrity of packaged BGA devices is tested by measuring electrical resistance using test sockets. Test sockets have been reported to often fail earlier than the expected life-time due to high contact resistance. This has been attributed to the formation of Sn oxide films on the Au coating layer of the probe pins loaded on the socket. Similar to contact failure, and known as "fretting", this process widely occurs between two conductive surfaces due to the continual rupture and accumulation of oxide films. However, the failure mechanism at the probe pin differs from fretting. In this study, the microstructural processes and formation mechanisms of Sn oxide films developed on the probe pin surface were investigated. Failure analysis was conducted mainly by FIB-FESEM observations, along with EDX, AES, and XRD analyses. Soft and fresh Sn was found to be transferred repeatedly from the solder bump to the Au surface of the probe pins; it was then instantly oxidized to SnO. The $SnO_2$ phase is a more stable natural oxide, but SnO has been proved to grow on Sn thin film at low temperature (< $150^{\circ}C$). Further oxidation to $SnO_2$ is thought to be limited to 30%. The SnO film grew layer by layer up to 571 nm after testing of 50,500 cycles (1 nm/100 cycle). This resulted in the increase of contact resistance and thus of signal delay between the probe pin and the solder bump.

Effect of BaF2 as a Flux in Solid State Synthesis of Y3Al5O12:Ce3+ (고상법을 이용한 Y3Al5O12:Ce3+의 제조에서 BaF2가 미치는 영향)

  • Won, Hyung-Seok;Hayk, Nersisyan;Won, Chang-Whan;Won, Hyung-Il
    • Korean Journal of Materials Research
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    • v.21 no.11
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    • pp.604-610
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    • 2011
  • The effect of $BaF_2$ flux in $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) formation was investigated. Phase transformation of $Y_3Al_5O_{12}$(YAG) was characterized by using XRD, SEM, and TEM-EDS, and it was revealed that the sequential formation of the $Y_4Al_2O_9$(YAM), $YAlO_3$(YAP) and $Y_3Al_5O_{12}$(YAG) in the temperature range of 1000-1500$^{\circ}C$. Single phase of YAG was revealed from 1300$^{\circ}C$. In order to find out the effect of $BaF_2$ flux, three modeling experiments between starting materials (1.5$Al_2O_3$-2.5$Y_2O_3$, $Y_2O_3$-$BaF_2$, and $Al_2O_3$-$BaF_2$) were done. These modeling experiments showed that the nucleation process occurs via the dissolution-precipitation mechanism, whereas the grain growth process is controlled via the liquid-phase diffusion route. YAG:Ce phosphor particles prepared using a proposed technique exhibit a spherical shape, high crystallinity, and an emission intensity. According to the experimental results conducted in this investigation, 5% of $BaF_2$ was the best concentration for physical, chemical and optical properties of $Y_3Al_5O_{12}:Ce^{3+}$(YAG:Ce) that is approximately 10-15% greater than that of commercial phosphor powder.

Hydroxyapatite prepared from eggshell and mulberry leaf extract by precipitation method

  • Wu, Shih-Ching;Hsu, Hsueh-Chuan;Hsu, Shih-Kuang;Liu, Mei-Yi;Ho, Wen-Fu
    • Biomaterials and Biomechanics in Bioengineering
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    • v.4 no.1
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    • pp.21-32
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    • 2019
  • Eggshell is a waste material after the usage of egg. In this work, biowaste chicken eggshells were used for preparing carbonated hydroxyapatite (HA) nanoparticles of high purity through aqueous precipitation method at room temperature. The eggshell-derived HA will be a cost-effective bioceramics for biomedical applications and an effective material-recycling technology. Additionally, mulberry leaf extract was used as a template to regulate the morphology, size and crystallinity of HA, and the effects of pH value were also examined. Characterization of the samples was performed by X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Scanning electron microscopy (SEM) was used to determine the size, shape and morphology of HA. The results indicate that only one phase of HA were synthesized in the both absence and presence of mulberry leaf extract at pH of 7 and above, while DCPD or DCPA/DCPD phase was observed at pH 4 condition. The crystallite sizes of the HA samples obviously decreased when adding mulberry leaf extract as a template, while they decreased gradually as the solution pH levels increased. With increasing pH level from 7 to 14, the rod-like HA nanoparticles gradually changed to spherical shape at pH 14. Note that, the obtained product is Mg and Sr containing A- and B-type carbonate HA at alkaline pH and it can be a potential material for biomedical applications.

PVA/H-β zeolite mixed matrix membranes for pervaporation dehydration of isopropanol-water mixtures

  • Huang, Zhen;Ru, Xiao-Fei;Guo, Yu-Hua;Zhu, Ya-Tong;Teng, Li-Jun
    • Membrane and Water Treatment
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    • v.10 no.2
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    • pp.165-178
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    • 2019
  • Mixed matrix membranes (MMMs) of poly (vinyl alcohol) (PVA) containing certain amounts of H-${\beta}$ zeolite for pervaporation were manufactured by using a solution casting protocol. These zeolite-embedded membranes were then characterized with scanning electron microscope (SEM), X-ray diffraction (XRD) and swelling tests. The membrane separation performance has been examined by means of isopropanol (IPA) dewatering from its highly concentrated aqueous solutions via response surface methodology (RSM). The results have demonstrated that the influences of feed IPA composition (85-95 wt.%), feed temperature ($50-70^{\circ}C$), zeolite loading (15-25 wt.%) and their interactive influences are all statistically significant on both pervaporation flux ($398-1228g/m^2{\cdot}h$) and water/isopropanol separation factor (617-2001). The quadratic models based on the RSM analysis have performed excellently to correlate experimental data with very high determination coefficients and very low relative standard deviations. The optimal pervaporation predictions given by using the RSM models demonstrate a total flux of $953g/m^2{\cdot}h$ and separation factor of 1458, and are excellently verified by experimental results. As reflected by these results, PVA MMMs embedded with hydrophilic $H-{\beta}$ zeolite entities have performed considerably better than its pure counterpart and indicated great potential for isopropanol dehydration applications.

Characteristics of Cu-Doped Ge8Sb2Te11 Thin Films for PRAM (PRAM용 Cu-도핑된 Ge8Sb2Te11 박막의 특성)

  • Kim, Yeong-Mi;Kong, Heon;Kim, Byung-Cheul;Lee, Hyun-Yong
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.32 no.5
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    • pp.376-381
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    • 2019
  • In this work, we evaluated the structural, electrical and optical properties of $Ge_8Sb_2Te_{11}$ and Cu-doped $Ge_8Sb_2Te_{11}$ thin films prepared by rf-magnetron reactive sputtering. The 200-nm-thick deposited films were annealed in a range of $100{\sim}400^{\circ}C$ using a furnace in an $N_2$ atmosphere. The amorphous-to-crystalline phase changes of the thin films were investigated by X-ray diffraction (XRD), UV-Vis-IR spectrophotometry, a 4-point probe, and a source meter. A one-step phase transformation from amorphous to face-centered-cubic (fcc) and an increase of the crystallization temperature ($T_c$) was observed in the Cu-doped film, which indicates an enhanced thermal stability in the amorphous state. The difference in the optical energy band gap ($E_{op}$) between the amorphous and crystalline phases was relatively large, approximately 0.38~0.41 eV, which is beneficial for reducing the noise in the memory devices. The sheet resistance($R_s$) of the amorphous phase in the Cu-doped film was about 1.5 orders larger than that in undoped film. A large $R_s$ in the amorphous phase will reduce the programming current in the memory device. An increase of threshold voltage ($V_{th}$) was seen in the Cu-doped film, which implied a high thermal efficiency. This suggests that the Cu-doped $Ge_8Sb_2Te_{11}$ thin film is a good candidate for PRAM.

Hot Corrosion Behavior of Plasma-Sprayed Partially Stabilized Zirconia Coatings in a Lithium Molten Salt (리튬용융염에서 플라즈마 용사된 부분안정화 지르코니아 코팅층의 고온부식 거동)

  • Cho, Soo-Haeng;Hong, Sun-Seok;Kang, Dae-Seong;Park, Byung-Heong;Hur, Jin-Mok;Lee, Han-Soo
    • Korean Journal of Metals and Materials
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    • v.46 no.10
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    • pp.646-651
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    • 2008
  • The electrolytic reduction of spent oxide fuel involves the liberation of oxygen in a molten LiCl electrolyte, which results in a chemically aggressive environment that is too corrosive for typical structural materials. It is essential to choose the optimum material for the process equipment handling molten salt. IN713LC is one of the candidate materials proposed for application in electrolytic reduction process. In this study, yttria-stabilized zirconia (YSZ) top coat was applied to a surface of IN713LC with an aluminized metallic bond coat by an optimized plasma spray process, and were investigated the corrosion behavior at $675^{\circ}C$ for 216 hours in the molten salt $LiCl-Li_2O$ under an oxidizing atmosphere. The as-coated and tested specimens were examined by OM, SEM/EDS and XRD, respectively. The bare superalloy reveals obvious weight loss, and the corrosion layer formed on the surface of the bare superalloy was spalled due to the rapid scale growth and thermal stress. The top coatings showed a much better hot-corrosion resistance in the presence of $LiCl-Li_2O$ molten salt when compared to those of the uncoated superalloy and the aluminized bond coatings. These coatings have been found to be beneficial for increasing to the hot-corrosion resistance of the structural materials for handling high temperature lithium molten salts.

Low Cost Alcoholic Breath Sensor Based on SnO2 Modified with CNTs and Graphene

  • Morsy, M.;Yahia, I. S.;Zahran, H.Y.;Ibrahim, M.
    • Journal of the Korean Physical Society
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    • v.73 no.10
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    • pp.1437-1443
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    • 2018
  • In this work, $SnO_2$ modified with reduced graphene oxide (rGO) and carbon nanotubes (CNTs) separately and combined sensitized by using the co-precipitation method and their sensing behavior toward ethanol vapor at room temperature were investigated. An interdigitated electrode (IDE) gold substrate is very expensive compared to a fluorine doped tin oxide (FTO) substrate; hence, we used the latter to reduce the fabrication cost. The structure and the morphology of the studied materials were characterized by using differential thermal analyses (DTA) and thermogravimetric analysis (TGA), transmission electron microscope (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Brunauer-Emmett-Teller surface area and Barrett-Joyner-Halenda (BJH) pore size measurements. The studied composites were subjected to ethanol in its gas phase at concentrations from 10 to 200 ppm. The present composites showed high-performance sensitivity for many reasons: the incorporation of $SnO_2$ and CNTs which prevents the agglomeration of rGO sheets, the formation of a 3D mesopourus structure and an increase in the surface area. The decoration with rGO and CNTs led to more active sites, such as vacancies, which increased the adsorption of ethanol gas. In addition, the mesopore structure and the nano size of the $SnO_2$ particles allowed an efficient diffusion of gases to the active sites. Based on these results, the present composites should be considered as efficient and low-cost sensors for alcohol.

IR Absorption Property in NaNo-thick Nickel Cobalt Composite Silicides (나노급 두께의 Ni50Co50 복합 실리사이드의 적외선 흡수 특성 연구)

  • Song, Oh Sung;Kim, Jong Ryul;Choi, Young Youn
    • Korean Journal of Metals and Materials
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    • v.46 no.2
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    • pp.88-96
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    • 2008
  • Thermal evaporated 10 nm-$Ni_{50}Co_{50}$/(70 nm-poly)Si films were deposited to examine the energy saving properties of silicides formed by rapid thermal annealing at temperature ranging from 500 to $1,100^{\circ}C$ for 40 seconds. Thermal evaporated 10 nm-Ni/(70 nm-poly)Si films were also deposited as a reference using the same method for depositing the 10 nm-$Ni_{50}Co_{50}$/(70 nm-poly)Si films. A four-point probe was used to examine the sheet resistance. Transmission electron microscopy (TEM) and X-ray diffraction XRD were used to determine cross sectional microstructure and phase changes, respectively. UV-VIS-NIR and FT-IR (Fourier transform infrared spectroscopy) were used to examine the near-infrared (NIR) and middle-infrared (MIR) absorbance. TEM analysis confirmed that the uniform nickel-cobalt composite silicide layers approximately 21 to 55 nm in thickness had formed on the single and polycrystalline silicon substrates as well as on the 25 to 100 nm thick nickel silicide layers. In particular, nickel-cobalt composite silicides showed a low sheet resistance, even after rapid annealing at $1,100^{\circ}C$. Nickel-cobalt composite silicide and nickel silicide films on the single silicon substrates showed similar absorbance in the near-IR region, while those on the polycrystalline silicon substrates showed excellent absorbance until the 1,750 nm region. Silicides on polycrystalline substrates showed high absorbance in the middle IR region. Nickel-cobalt composite silicides on the poly-Si substrates annealed at $1,000^{\circ}C$ superior IR absorption on both NIR and MIR region. These results suggest that the newly proposed $Ni_{50}Co_{50}$ composite silicides may be suitable for applications of IR absorption coatings.

Effect of Heat Treatment on the Mechanical Properties of a Ti-15Mo-3Nb-3Al-0.2Si Alloy (β-type Ti-14Mo-3Nb-3Al-0.2Si 합금의 열처리 조건에 따른 기계적 특성)

  • Kim, Tae Ho;Lee, Jun Hee;Hong, Sun Ig
    • Korean Journal of Metals and Materials
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    • v.49 no.2
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    • pp.121-127
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    • 2011
  • The mechanical properties of the various heat treatment conditions on Ti-15Mo-3Nb-3Al-0.2Si alloy plates were examined. XRD patterns from the surface of Ti-15Mo-3Nb-3Al-0.2Si were analyzed as a solution-treated Ti alloy has the single-phase ${\beta}$ structure whereas the aged Ti alloys have the ${\beta}$ matrix embedded with ${\alpha}$ needles. High strength (~1500 MPa) with decent ductility (7%) was obtained by the Ti alloy double aged at $300^{\circ}C$ and $520^{\circ}C$ for 8 hours each. The double-aged alloy exhibits the finer structure than the single-aged alloy at $300^{\circ}C$ for 8 hours because of the higher nucleation rate of ${\alpha}$ needles at an initial low aging temperature ($320^{\circ}C$). TEM observation revealed that the fine nanostructure with ${\alpha}$ needles in the ${\beta}$ matrix ensured the excellent mechanical properties in the double aged Ti-15Mo-3Nb-3Al-0.2Si alloy. In the solution treated alloy, the yield drop, stress-serrations and the ductility minimum typically associated with dynamic strain aging can be attributed to the dynamic interaction between dislocations and oxygen atoms. The yield drop and the stress serration were not observed in aged samples because the geometrically introduced dislocations due to phase precipitates suppressed the dynamic strain aging.

Characterization and thermophysical properties of Zr0.8Nd0.2O1.9-MgO composite

  • Nandi, Chiranjit;Kaity, Santu;Jain, Dheeraj;Grover, V.;Prakash, Amrit;Behere, P.G.
    • Nuclear Engineering and Technology
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    • v.53 no.2
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    • pp.603-610
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    • 2021
  • The major drawback of zirconia-based materials, in view of their applications as targets for minor actinide transmutation, is their poor thermal conductivity. The addition of MgO, which has high thermal conductivity, to zirconia-based materials is expected to improve their thermal conductivity. On these grounds, the present study aims at phase characterization and thermophysical property evaluation of neodymium-substituted zirconia (Zr0.8Nd0.2O1.9; using Nd2O3 as a surrogate for Am2O3) and its composites with MgO. The composite was prepared by a solid-state reaction of Zr0.8Nd0.2O1.9 (synthesized by gel combustion) and commercial MgO powders at 1773 K. Phase characterization was carried out by X-ray diffraction and the microstructural investigation was performed using a scanning electron microscope equipped with energy dispersive spectroscopy. The linear thermal expansion coefficient of Zr0.8Nd0.2O1.9 increases upon composite formation with MgO, which is attributed to a higher thermal expansivity of MgO. Similarly, specific heat also increases with the addition of MgO to Zr0.8Nd0.2O1.9. Thermal conductivity was calculated from measured thermal diffusivity, temperature-dependent density and specific heat values. Thermal conductivity of Zr0.8Nd0.2O1.9-MgO (50 wt%) composite is more than that of typical UO2 fuel, supporting the potential of Zr0.8Nd0.2O1.9-MgO composites as target materials for minor actinides transmutation.