• Journal of the Mineralogical Society of Korea
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• v.13 no.2
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• pp.53-64
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• 2000

Chlorite from the talc deposits in the Chungnam area, Korea, has been studied using electron microprobe analysis and high resolution transmission electron microscopy (HRTEM), Talc orea are hydrothermal alteration products of serpentinite which was originated from ultramafic rocks. Chlorite occurs in close association with talc ores of with the black alteration zone between talc ore bodies and granitic gneiss. It is the most abundant impurity mineral of talc ores. Chlorite in association with talc is characterized by very high but narrow variation in Mg/(Mg+Fe) ratios (0.784~0.951), significant octahedral substitution (-0.200~0.692), wide variation in Al contents (1.085~3.160 / 14 oxygens), and high Cr and Ni contents. It was formed under a very limited but high Mg/(Mg+Fe) condition in close connection with serpentinite. Chlorite in the black alteration zone is characterized by a high Fe content, wide variation in Mg/(Mg+Fe) ratios (0.378~0.852), narrow octahedral substitution (-0.035~0.525), high narrow Al contents (1.468~2.959), and low Cr and Ni contents. It was formed under a low Mg/(Mg+Fe) and relatively Al-rich condition in close connection with county rocks. Two different chemical modes for chlorite suggest two different origins for two different chlorites. Although most of chlorites show typical 14-$\AA$ lattice fringe images under HRTEM, some chlorites show fringe images of 21-$\AA$ (14$\AA$+7$\AA$) spacings within (001) lattice-fringe images of chlorite (14$\AA$). But brown chlorite from the black zone has high Ti and K contents suggesting that mica was the precursor of brown chlorite. Such possibility is also supported by the fact that lattice-fringe images of brown chlorite show 14-$\AA$ chlorite layers in which 10-$\AA$ mica single layer or packets are interlayered. Partial terminations from 3 mica layers to 2 chlorite layers are often observed. It, therefore, is suggested that the chlorite associated with talc ores is a hydrothermal alteration products of serpentinite, whereas the chlorites in the black alteration zone is a hydrothermal alteration product of granitic gnesis under a partial influence of serpentinite.

• Journal of Welding and Joining
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• v.30 no.1
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• pp.64-71
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• 2012

The characteristics of high heat input (342kJ/cm) EG (Electro Gas Arc) welded joint of EH36-TM steel has been investigated. The weld metal microstructure consisted of fine acicular ferrite (AF), a little volume of polygonal ferrite (PF) and grain boundary ferrite (GBF). Charpy impact test results of the weld metal and heat affected zone (HAZ) met the requirement of classification rule (Min. 34J at $-20^{\circ}C$). In order to evaluate the relationship between the impact toughness property and the grain size of HAZ, the austenite grain size of HAZ was measured. The prior austenite grain size in Fusion line (F.L+0.1 mm) was about $350{\mu}m$. The grain size in F.L+1.5 mm was measured to be less than $30{\mu}m$ and this region was identified as being included in FGHAZ(Fine Grain HAZ). It is seen that as the austenite grain size decreases, the size of GBF, FSP (Ferrite Side Plate) become smaller and the impact toughness of HAZ increases. Therefore, the CGHAZ was considered to be area up to 1.3mm away from the fusion line. Results of TEM replica analysis for a welded joint implied that very small size ($0.8\sim1.2{\mu}m$) oxygen inclusions played a role of forming fine acicular ferrite in the weld metal. A large amount of (Ti, Mn, Al)xOy oxygen inclusions dispersed, and oxides density was measured to be 4,600-5,300 (ea/mm2). During the welding thermal cycle, the area near a fusion line was reheated to temperature exceeding $1400^{\circ}C$. However, the nitrides and carbides were not completely dissolved near the fusion line because of rapid heating and cooling rate. Instead, they might grow during the cooling process. TiC precipitates of about 50 ~ 100nm size dispersed near the fusion line.

• Journal of the Korean Association of Oral and Maxillofacial Surgeons
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• v.30 no.1
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• pp.1-16
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• 2004

The use of artificial nerve conduit containing viable Schwann cells is one of the most promising strategies to repair the peripheral nerve injury. To fabricate an effective nerve conduit whose microstructure and internal environment are more favorable in the nerve regeneration than existing ones, a new three-dimensional Schwann cell culture technique using $Matrigel^{(R)}$. and dorsal root ganglion (DRG) was developed. Nerve conduit of three-dimensionally arranged Schwann cells was fabricated using direct seeding of freshly harvested DRG into a $Matrigel^{(R)}$ filled silicone tube (I.D. 1.98 mm, 14 mm length) and in vitro rafting culture for 2 weeks. The nerve regeneration efficacy of three-dimensionally cultured Schwann cell conduit (3D conduit group, n=6) was assessed using SD rat sciatic nerve defect of 10 mm, and compared with that of silicone conduit filled with $Matrigel^{(R)}$ and Schwann cells prepared from the conventional plain culture method (2D conduit group, n=6). After 12 weeks, sciatic function was evaluated with sciatic function index (SFI) and gait analysis, and histomorphology of nerve conduit and the innervated tissues of sciatic nerve were examined using image analyzer and electromicroscopic methods. The SFI and ankle stance angle (ASA) in the functional evaluation were $-60.1{\pm}13.9$, $37.9^{\circ}{\pm}5.4^{\circ}$ in 3D conduit group (n=5) and $-87.0{\pm}12.9$, $32.2^{\circ}{\pm}4.8^{\circ}$ in 2D conduit group (n=4), respectively. And the myelinated axon was $44.91%{\pm}0.13%$ in 3D conduit group and $13.05%{\pm}1.95%$ in 2D conduit group to the sham group. In the TEM study, 3D conduit group showed more abundant myelinated nerve fibers with well organized and thickened extracellular collagen than 2D conduit group, and gastrocnemius muscle and biceps femoris tendon in 3D conduit group were less atrophied and showed decreased fibrosis with less fatty infiltration than 2D conduit group. In conclusion, new three-dimensional Schwann cell culture technique was established, and nerve conduit fabricated using this technique showed much improved nerve regeneration capacity than the silicone tube filled with $Matrigel^{(R)}$ and Schwann cells prepared from the conventional plain culture method.

• Journal of Welding and Joining
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• v.33 no.5
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• pp.26-30
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• 2015

Hastelloy X in this study was applied in jet engine F-15 air fighter as shroud to isolate the engine from outer skin. After 15 years operation at elevated temperature the mechanical properties decreased gradually due to the precipitation of continues second phases in the grain boundaries and precipitated inside the grain. The crack happened at the edge of the shroud due to the thermal and mechanical stress from jet engine. Selective TEM analysis found that the grain boundaries consist of $M_{23}C_6$ carbide, $M_6$ Ccarbide and small percentage of sigma(${\sigma}$) phase. Furthermore, it was confirmed the nano size of ${\sigma}$ and miu (${\mu}$) phase inside the grain. In this study, it was investigated the microstructure of the degraded shroud component and HAZ of repair welded shroud. In the HAZ, it was observed the dissolution of the $M_{23}C_6$ carbides and smaller precipitates, the migration of the undissolved larger $M_{23}C_6$ carbide and $M_6$ Ccarbide. It is also observed the liquation due to the simply melt of the segregated precipitates in the grain boundaries. Interestingly, the segregated second phases which simply melt in the grain boundaries more easily happened at higher heat input welding condition. High temperature tensile test was done at $300^{\circ}C$, $700^{\circ}C$ and $900^{\circ}C$. It was obtained that the toughness of welded sample is lower compare to the non-welded sample. The solution heat treatment at $1170^{\circ}C$ for 5 minutes was suggested to obtain a better mechanical properties of the shroud. The high cycle fatigue number of the repair welded shroud shows a much lower compare to the shroud. In addition, the high cycle fatigue number at room temperature after solution heat treatment was almost double compare to the before solution heat treatment under 420-500MPa stress amplitude. However, the high cycle fatigue number of repaired welded sample was shown a much lower compare to the non- welded shroud and solution treated shroud. One of the main reasons to decrease the tensile strength and the high cycle fatigue properties of the repair welded shroud is the formation of the liquid phase in HAZ.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.6 no.6
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• pp.457-460
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• 2005

Nano-sized titanium oxide and zirconium oxide powders were synthesized by hydrolysis of titanium isopropoxide $[Ti(OC_3H7)_4]$ and zirconium tetrachloride ($ZrC1_4$) via a sol-gel technique. Lead titanate powders were prepared by mixing $TiO_2$ precursors with PbO slurry made with dilute $NH_4OH$. Lead zirconate titanate powders were, then, synthesized by mixing $PbTiO_3$ with $ZrO_2$ powders. The goal of this research was to obtain the $PbZrTiO_3(PZT)$ powders and sintering these powders at low temperature. The $PbTiO_3$ and PZT powders after firing were analyzed by X-ray diffraction(XRD) and transmission electron microscopy(TEM) was utilized to observe the shape and size of the synthesized nano-particles. In the XRD pattern, the well-crystallized PZT phase could be obtained in consequence of firing at $900^{\circ}C$. SEM micrographs also showed that grains of PZT were relatively well grown with the size of the range of $2{\~}4{\mu}m$. The densified perovskite structure of $PbZrTiO_3$ could be obtained by sintering at temperature as low as $900^{\circ}C$. Characterization of the samples showed improved piezoelectric properties.

• Journal of Powder Materials
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• v.13 no.5 s.58
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• pp.327-335
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• 2006

In the development of new hydrogen absorbing materials for a next generation of metal hydride electrodes for rechargeable batteries, metastable Mg-Ni-based compounds find currently special attention. Amor phous-nanocrystalline $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ alloys were produced by mechanical alloying and melt-spinning and characterized by means of XRD, TEM and DSC. On basis of mechanically alloyed Mg-Ni-Y powders, complex hydride electrodes were fabricated and their electrochemical behaviour in 6M KOH (pH=14,8) was investigated. The electrodes made from $Mg_{63}Ni_{30}Y_7$ powders, which were prepared under use of a SPEX shaker mill, with a major fraction of nanocrystalline phase reveal a higher electrochemical activity far hydrogen reduction and a higher maximum discharge capacity (247 mAh/g) than the electrodes from alloy powder with predominantly amorphous microstructure (216 mAh/g) obtained when using a Retsch planetary ball mill at low temperatures. Those discharge capacities are higher that those fur nanocrystalline $Mg_2Ni$ electrodes. However, the cyclic stability of those alloy powder electrodes was low. Therefore, fundamental stability studies were performed on $Mg_{63}Ni_{30}Y_7$ and $Mg_{50}Ni_{30}Y_{20}$ ribbon samples in the as-quenched state and after cathodic hydrogen charging by means of anodic and cathodic polarisation measurements. Gradual oxidation and dissolution of nickel governs the anodic behaviour before a passive state is attained. A stabilizing effect of higher fractions of yttrium in the alloy on the passivation was detected. During the cathodic hydrogen charging process the alloys exhibit a change in the surface state chemistry, i.e. an enrichment of nickel-species, causing preferential oxidation and dissolution during subsequent anodization. The effect of chemical pre-treatments in 1% HF and in $10\;mg/l\;YCl_3/1%\;H_2O_2$ solution on the surface degradation processes was investigated. A HF treatment can improve their anodic passivation behavior by inhibiting a preferential nickel oxidation-dissolution at low polarisation, whereas a $YCl_3/H_2O_2$ treatment has the opposite effect. Both pre-treatment methods lead to an enhancement of cathodically induced surface degradation processes.

• Journal of the Microelectronics and Packaging Society
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• v.13 no.1 s.38
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• pp.1-5
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• 2006

We prepared 80 nm-thick TiSix on each 70 nm-thick amorphous silicon and polysilicon substrate using an RF sputtering with $TiSi_2$ target. TiSix composite silicide layers were stabilized by rapid thermal annealing(RTA) of $800^{\circ}C$ for 20 seconds. Line width of $0.5{\mu}m$ patterns were embodied by photolithography and dry etching process, then each additional annealing process at $750^{\circ}C\;and\;850^{\circ}C$ for 3 hours was executed. We investigated the change of sheet resistance with a four-point probe, and cross sectional microstructure with a field emission scanning electron microscope(FE-SEM) and transmission electron microscope(TEM), respectively. We observe an abrupt change of resistivity and voids at the silicide surface due to interdiffusion of silicide and composite titanium silicide in the amorphous substrates with additional $850^{\circ}C$ annealing. Our result implies that the electrical resistance of composite titanium silicide may be tunned by employing appropriate substrates and annealing condition.

• Journal of the Microelectronics and Packaging Society
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• v.21 no.3
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• pp.25-29
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• 2014

Plasma organic thin film for PCB surface finish is a potential replacement of the conventional PCB finishes because of environment-friendly process, high corrosion-resistance and long shelf life over 1 year. In this study, solder joint properties of the plasma organic surface finish were estimated and compared with OSP surface finish. The plasma surface finish was deposited by chemical vapor deposition from fluorine-based precursors. The thickness of the plasma organic coating was 20 nm. Sn-3.0Ag-0.5Cu (SAC305) solder was used as solder joint materials. From a salt spray test, the plasma organic coating had higher corrosion resistance than the OSP surface finish. The spreadability of SAC305 on plasma organic coating was higher than that on OSP surface finish. SEM and TEM micrographs showed that the interfacial microstructure of the plasma surface finish sample were similar to that of the OSP sample. Solder joint strength of the plasma finish sample was also similar to that of the OSP finished sample.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.327.1-327.1
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• 2014

Nitrides-on-silicon structures are considered to be an excellent candidate for unique design architectures and creating devices for high-power applications. Therefore, a lot of effort has been concentrating on growing high-quality III-nitrides on Si substrates, mostly Si(111) and Si(001) substrates. However, there are several fundamental problems in the growth of nitride compound semiconductors on silicon. First, the large difference in lattice constants and thermal expansion coefficients will lead to misfit dislocation and stress in the epitaxial films. Second, the growth of polar compounds on a non-polar substrate can lead to antiphase domains or other defective structures. Even though the lattice mismatches are reached to 16.9 % to GaN and 19 % to AlN and a number of dislocations are originated, Si(111) has been selected as the substrate for the epitaxial growth of nitrides because it is always favored due to its three-fold symmetry at the surface, which gives a good rotational matching for the six-fold symmetry of the wurtzite structure of nitrides. Also, Si(001) has been used for the growth of nitrides due to a possible integration of nitride devices with silicon technology despite a four-fold symmetry and a surface reconstruction. Moreover, Si(110), one of surface orientations used in the silicon technology, begins to attract attention as a substrate for the epitaxial growth of nitrides due to an interesting interface structure. In this system, the close lattice match along the [-1100]AlN/[001]Si direction promotes the faster growth along a particular crystal orientation. However, there are insufficient until now on the studies for the growth of nitride compound semiconductors on Si(110) substrate from a microstructural point of view. In this work, the microstructural properties of nitride thin layers grown on Si(110) have been characterized using various TEM techniques. The main purpose of this study was to understand the atomic structure and the strain behavior of III-nitrides grown on Si(110) substrate by molecular beam epitaxy (MBE). Insight gained at the microscopic level regarding how thin layer grows at the interface is essential for the growth of high quality thin films for various applications.

• Proceedings of the KWS Conference
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• 2009.11a
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• pp.72-72
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• 2009

전자부품의 내부접속 및 파워반도체의 다이본딩과 같은 1차실장에는 고온환경에서의 사용과 2차실장에서의 재용융방지를 위해 높은 액상선온도 및 고상선온도를 필요로 하여, Pb-5wt%Sn, Pb-2.5wt%Ag로 대표되는 납성분 85%이상의 고온솔더가 널리 사용되고 있다. 생태계와 인체에 대한 납의 유해성이 보고된 이래, 무연솔더에 대한 연구가 활발히 진행되어 왔으나, Sn-Ag-Cu계로 대표되는 Sn계 합금으로 대체 중인 중온용 솔더와는 달리, 고온용 솔더에 대해서는 대체합금에 대한 연구가 미흡한 실정이다. 대체재의 부재로 인해 기존의 납을 다량함유한 솔더로 1차실장이 지속됨으로서, 2차실장의 무연화에도 불구하고 전자부품 및 기기의 재활용에 큰 어려움을 겪고 있다. 지금까지 고온용 무연솔더로서는 융점에 근거해 Au-(Sn, Ge, Si)계, Bi-Ag계, Zn-(Al, Sn)계의 극히 제한된 합금계만이 보고되어 왔다. Au계 솔더는 현재 플럭스를 사용하지 않는 광학, 디스플레이 분야 등 고부가가치 공정에 사용되고 있으나, 합금가격이 매우 비싸며 가공성이 나빠 대체재료로서는 적합하지 않다. Bi-Ag계 솔더 또한 취성합금으로 와이어 및 박판으로 가공하는데 어려움이 크며, 솔더로서 중요한 특성중 하나인 전기전도도 및 열전도도가 나쁜 편이다. 이에 비해, Zn계 합금은 비교적 낮은 합금가격, 적절한 가공성과 뛰어난 인장강도, 우수한 전기전도도 및 열전도도를 지녀, 고온용솔더 대체재료의 유력한 후보로 생각된다.이전 연구에서, 필자의 연구그룹은 Zn-Sn계 합금을 고온용 무연솔더로서 제안한 바 있다. Zn-Sn계 합금은 충분히 높은 융점과 함께, 금속간화합물이 없는 미세조직, 우수한 기계적 특성, 높은 전기전도도 및 열전도도 등의 장점을 나타내었다. 본 연구에서는 기초합금특성상 고온솔더로서 다양한 장점을 지닌 Zn-30wt%Sn합금을 고온용 솔더의 대표적인 적용의 하나인 다이본딩에 적용하여, 접합부의 강도 및 미세조직, 열피로 신뢰성에 대해 분석을 함으로서 실제 공정에의 적용가능성에 대해 검토하였다. Zn-30wt%Sn을 이용해 Au/TiN(Titanium nitride) 코팅한 Si다이를 AlN-DBC(aluminum nitride-direct bonded copper)기판에 접합한 결과, 양측에 완전히 젖은 기공이 없는 양호한 다이접합부를 얻었으며, 솔더내부에는 금속간화합물을 형성하지 않았다. Si다이와의 계면에는 TiN만이 존재하였으며, Cu와의 계면에는 Cu로부터 $Cu_5Zn_8,\;CuZn_5$의 반응층을 형성하였다. 온도사이클시험을 통한 열피로특성평가에서, Zn-30wt%Sn를 이용한 다이접합부는 1500사이클 지점에서 Cu와 Cu-Zn금속간화합물의 사이에서 피로균열이 형성되며, 접합강도가 크게 감소하였다. 열피로특성 향상을 위해 Cu표면에 TiN코팅을 하여 Zn-30wt%Sn 솔더로 다이접합한 결과, Si다이와 기판 양측에 TiN만으로 구성된 계면을 형성하였으며, TEM관찰을 통해 Zn-30wt%Sn과 극히 미세한 접합계면이 형성하고 있음을 확인하였다. Zn-wt%30Sn솔더와 TiN층의 병용으로 2000사이클까지 미세조직의 변화 및 강도저하가 없는 극히 안정된 고신뢰성의 다이접합부를 얻을 수가 있었다.