• Journal of the Korean Vacuum Society
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• v.11 no.3
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• pp.176-182
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• 2002

Amorphous $TiO_2$ thin films were deposited on glass substrates by ion beam sputtering in which the ratio of $O_2$/Ar gas used as discharged gas was varied from 0 to 2. After optical and microstructure properties and chemical composition of thin films was analyzed, antireflection coating layers were fabricated with $SiO_2$/$TiO_2$ multi-layers. Thin films deposition was performed at room temperature and ion beam voltage and ion current density for sputtering of target were fixed at 1.2 kV and 200 $\mu\textrm{A}/\textrm{cm}^2$, respectively. Refractive indexs of the deposited $TiO_2$films were 2.40-2.45 at a wavelength of 633 nm. $TiO_2$films had high transmission and stoichiometry when ratio of $O_2$/Ar was 1. Rms roughness of deposited $TiO_2$ film was below 7 $\AA$. In excessive $O_2$ environments, however Rms roughness increased over 50 $\AA$. Transmittance decreased by scattering of rough surface. Reflectance of $SiO_2$/$TiO_2$multi-layers was below 1% in visible light.

• 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.

• Proceedings of the KWS Conference
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• 2009.11a
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• pp.49-49
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• 2009

마찰교반접합법은 특정한 회전수로 회전하는 용접 툴을 이용하여 접합하고자 하는 피접합재의 맞댄면에 삽입시킨 후 툴을 이동시키거나 혹은 시편을 견고하게 고정시킨 장치(backing plate)가 움직여 고상 상태에서 접합이 이루어진다. 알루미늄, 마그네슘 등 비교적 융점이 낮은 저융점 재료의 재료에 처음 적용이 되어 많은 연구가 활발히 진행되었고 타 용접방법에 비해 우수한 접합특성을 나타내었다. 최근 이러한 마찰교반접합은 이러한 저융점 재료를 넘어서 스틸, 타이타늄, 니켈 등과 같은 고융점 재료 등에 대한 적용이 늘어나고 있다. 마찰교반접합을 이용하여 이러한 고융점 재료의 접합 경우 내마모성 및 내열성 등의 내구성이 갖추어진 툴과 이러한 툴을 냉각시킬 수 있는 냉각 장치 등이 필요로 하나 경제적 측면이나 접합부의 우수한 특성 등을 고려 할 때 그 적용 및 발전 가능성이 매우 높다고 볼 수 있다. 최근 무공해 연료로 각광받고 있는 액화천연가스 (LNG)의 수요가 급증함에 따라 LNG 저장탱크 소재로 널리 사용되고 있는 9% Ni강의 수요 또한 증가하고 있는 상황이다. 하지만 9% Ni 강은 극저온용 소재로 용접부의 저온인성 ($-196^{\circ}C$)이 가장 중요하기 때문에 저온인성을 확보하고자 Inconel 계나 Hastelloy계 등의 니켈 기 합금을 용접재료로 사용하고 있으나 이러한 용접재료는 가격이 매우 고가이며 또한 용접 후 용접부의 강도가 낮다는 문제가 제기되고 있다. 또한 LNG 탱크 제작시 사용되는 용접법은 GTAW, SAW 및 SMAW 이지만 국내에서는 주로 SMAW에 의존하고 있는 실정인 관계로 보다 더 경제적인 용접 프로세스의 적용 가능성이 검토되고 있는 상황이다. 본 연구에서는 마찰교반용접을 이용하여 두께 4mm의 9% Ni 강에 대해 맞대기 마찰교반접합을 실시하였다. 툴 회전 속도 및 접합 속도를 고정한 상태에서 접합을 실시 하였으며 접합 시 툴은 $Si_3N_4$로 제작된 툴을 사용하였다. 접합 후 외관상태 점검, 미세조직 관찰, 경도, 인장 강도 및 저은 충격 측정 등의 실험을 실시하였고, 이러한 결과를 이용하여 미세조직과 기계적 특성과의 관련성을 조사하였다.

• Journal of the Korean Society for Nondestructive Testing
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• v.21 no.4
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• pp.439-445
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• 2001

The destructive method is reliable and widely used lot the estimation of material degradation but, it have time-consuming and a great difficulty in preparing specimens from in-service industrial facilities. Therefore, the estimation of degraded structural materials used at high temperature by nondestructive evaluation such as electric resistance method, replica method, Barkhausen noise method, electro-chemical method and ultrasonic method are strongly desired. Ultrasonic nondestructive evaluation technique has been reported good to attain efficiency of measurement, high sensitivity of measurement, and rapidity and reliability of result interpretation. In this study, it was verified experimentally the feasibility of the evaluation of degraded 2.25Cr-1Mo steel specimens which were prepared by the isothermal aging heat treatment at $630^{\circ}C$ by high frequency longitudinal wave method investigating the change of attenuation coefficient by FFT analysis and wavelet transform. Because of carbide precipitation increase and spheroidization near grain boundary of microstructure to aging degradation, attenuation coefficient had a tendency to increase as degradation proceeded. It was identified possibly to evaluate degradation using the characteristics of high-frequency ultrasonics. Frequency dependence of ultrasonic attenuation coefficient to aging degradation appeared large, which made sure that attenuation coefficient is an important parameter for evaluation of aging degradation.

• Journal of the Korean Vacuum Society
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• v.17 no.5
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• pp.466-472
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• 2008

Purple Gold is the alloy consisting of 78wt%Au-22wt%Al, and is expressed as a chemical formula, $AuAl_2$. Lately it is being used for the material of accessories or the decorative ornaments, being one of the colored golds having the peculiar purple color, like White Gold and Pink Gold. Purple Gold has the weak point in shaping through casting process due to the bad malleability and castability, being the intermetalic compound of Au and Al. Therefore, it is possible to produce the final product only by the cutting and the grinding process or to use it as a decorative coat with the thin film evaporation. This study implemented two kinds of thin film experiments. One is the case that heat treatment was made after Au and Al deposition evaporated separately with a weight ratio 78:22 on the 200nm$SiO_2$/Si substrate. The other is the case that the surface deposition was made through the vacuum evaporation, keeping the glass substrate temperature remain room temperature, using the bulk $AuAl_2$ as a source. The final film property was measured, focusing on the Purple Gold's color and thickness through the bare eye inspection, the microstructure analysis, the surface resistance analysis, the color difference analysis, and XRD analysis. Purple Gold was not formed, as the excessive surface agglomeration occurred, in case of being produced and treated thermally with 12.5nmAu/40nmAl/200nm$SiO_2$/Si structure. Our results suggest that of Purple Gold films, showing the same purple color as the bulk's, were successfully deposited with the direct thermal evaporation from the $AuAl_2$ bulk source.

• Korean Journal of Materials Research
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• v.13 no.9
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• pp.572-580
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• 2003

Synthesizing behavior and microstructural evolution of $CaZrO_3$and $m-ZrO_2$in a thermal reaction process of $ZrSiO_4$-$xCaCO_3$mixtures, where x is 7 and 19, were investigated to determine the addition amount of CaO in CaO:$ZrO_2$:$SiO_2$ternary composition. CaZrO$_3$-Ca$_2$SiO$_4$precursor prepared by the mixture of $ZrSiO_4$and CaCO$_3$in aqueous suspending media was controlled to the acidic (pH=4.0) condition with HCI solution to enhance the thermal reaction. The addition amount of dispersant into the $ZrSiO_4$-$xCaCO_3$slip increased with increasing mole ratio of $CaCO_3$, which was associated with the viscosity of slip. Decarbonation reaction was activated with an increase of the addition amount of $CaCO_3$, showing different final temperatures in $ZrSiO_4$-$7CaCO_3$and $ZrSiO_4$-$19CaCO_3$mixtures as about 980 and 116$0^{\circ}C$, respectively, for finishing decarbonation reaction. The grain morphology was changed to spherical shape for all samples with an increase of sintering temperature. The grain size and phase composition of the synthesized composites depended on the mixture ratio of Zrsi04 and CacO3 powders, indicating that the main crystals were m-ZrO2 ($\leq$3 $\mu\textrm{m}$) and $CaZrO_3$ ($\leq$ 7 $\mu\textrm{m}$) in $ZrSiO_4$$>-7CaCO_3$and $ZrSiO_4$-$19CaCO_3$mixtures, respectively.

• Journal of Powder Materials
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• v.24 no.2
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• pp.133-140
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• 2017

This study investigates the oxidation properties of Fe-14Cr ferritic oxide-dispersion-strengthened (ODS) steel at various high temperatures (900, 1000, and $1100^{\circ}C$ for 24 h). The initial microstructure shows that no clear structural change occurs even under high-temperature heat treatment, and the average measured grain size is 0.4 and $1.1{\mu}m$ for the as-fabricated and heat-treated specimens, respectively. Y-Ti-O nanoclusters 10-50 nm in size are observed. High-temperature oxidation results show that the weight increases by 0.27 and $0.29mg/cm^2$ for the as-fabricated and heat-treated ($900^{\circ}C$) specimens, and by 0.47 and $0.50mg/cm^2$ for the as-fabricated and heat-treated ($1000^{\circ}C$) specimens, respectively. Further, after 24 h oxidation tests, the weight increases by 56.50 and $100.60mg/cm^2$ for the as-fabricated and heat-treated ($1100^{\circ}C$) specimens, respectively; the latter increase is approximately 100 times higher than that at $1000^{\circ}C$. Observation of the surface after the oxidation test shows that $Cr_2O_3$ is the main oxide on a specimen tested at $1000^{\circ}C$, whereas $Fe_2O_3$ and $Fe_3O_4$ phases also form on a specimen tested at $1100^{\circ}C$, where the weight increases rapidly. The high-temperature oxidation behavior of Fe-14Cr ODS steel is confirmed to be dominated by changes in the $Cr_2O_3$ layer and generation of Fe-based oxides through evaporation.

• Journal of Conservation Science
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• v.36 no.5
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• pp.421-429
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• 2020

This study examined the manufacturing process of a furnace wall excavated from the Songdu-ri Site in Jincheon, and the difference in material composition between the 11 layers of the wall using physicochemical analyses. Based on microstructure observations, these layers could be largely divided into three groups: an undercalcined first layer, calcined second to ninth layer with evidences of partial heat, and non-fired soil layers from the tenth to the eleventh layer. Particle size analyses revealed that the fired layer constituted a relatively higher content of coarse sand than the non-fired layer. This difference was further confirmed by the results of the curvature coefficient analysis. An analysis of the constituent minerals showed similar overall XRD diffraction patterns between the different layers, but variations in the intensity of the low-temperature and high-temperature minerals. This indicates that the degree of heat was different. The thermal analysis results demonstrated that the heating peak of mullite was only reached in the first and second layers of the wall, thus implying these as the layers to be finally used. Consequently, no significant difference could be observed between the materials of the various layers of the wall. Thus, it can be suggested that the furnace wall was constructed using clay, which had a composition similar to that of the soil present in the area. However, the shape and characteristics of the constituent particles between the layers displayed partial variations, and it is possible that some external materials might have been added.

• Journal of Sensor Science and Technology
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• v.10 no.2
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• pp.101-107
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• 2001

A highly selective, sensitive and reliable ozone sensing $In_2O_3$ thin film was fabricated by a sol-gel method. The fabricated film is operated at a relatively lower temperature than ever developed thin films and saved operating power. $In_2O_3$ films deposited by sol-gel technique has been recently attracted because it is an economical and energy saving method and precisely controlled microstructure. Indium alkoxide precursor was synthesized from the reaction between indium hydroxide and butanol. PVA binder was used to improve adhesion of the films. The $In_2O_3$ thin films were obtained by spin coating from 1 to 5 times followed by drying at $100^{\circ}C$ and calcining at $600^{\circ}C$ for 1h. The film thickness was controlled by the number of coating time. The morphology and the thickness of the $In_2O_3$ films were examined by a SEM and XRD. The $In_2O_3$ thin films show a high sensitive to ozone gas at operating temperature of $250^{\circ}C$. The $In_2O_3$ sensor has very good selectivity to $CH_4$, CO, $C_4H_{10}$ and ethanol.

• Applied Chemistry for Engineering
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• v.8 no.6
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• pp.994-999
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• 1997

The sintering properties of hydroxyapatite isolated from tuna bone and hydroxyapatite-containing wollastonite sintered by solid-state reaction was investigated. As the sinterability of hydroxyapatite dependent upon the particle size by dry milling, it showed a sintering. But the hydroxyapatite-containing wollastonite was appeared good sinterability. On X-ray measurements, the major phases of hydroxyapatite-containing wollastonite by solid state reaction at $1250^{\circ}C$ were identified as hydroxyapatite and pseudowollastonite(${\alpha}-CaSiO_3$). And the phases appeared as whitlockite [$Ca_3(PO_4)_2$] by decomposition of hydroxyapatite at higher temperature above $1250^{\circ}C$. The shapes of microstructure on SEM images changed from porous to dense bulk by elevating temperature. The mean bending strength of hydroxyapatite-containing wollastonite sintered by solid-state reaction at $1300^{\circ}C$ was about 18 MPa, it was close to the cancellous bone's maximum strength, 20 MPa.