• Proceedings of the Materials Research Society of Korea Conference
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• 2011.10a
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• pp.26-26
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• 2011

Fe계 TiC 합금은 미량의 합금원소를 첨가시켜 경화능, 내식성, 내마모성 성질을 개선한 특수 공구용 재료로서 현재 절삭, 내마모성, 광산, 금형재료 등의 분야에 널리 사용되고 있다. 금속과 세라믹의 복합재료인 초경합금은 비열처리용 공구강으로 WC, TiC 등의 4, 5, 6족 금속탄화물에 Co, Ni, Fe등의 철족이 결합금속으로 소결한 복합재료로 WC-Co계 초경합금이 주종을 이루고 있으나, 전략 소재로서 고가인 Co 원료를 대체하기 위한 재료로서 초경재료의 고경도와 공구강의 경제성 및 가공성의 장점을 이용한 Fe-TiC계 초경합금의 연구가 다양하게 진행되고 있다. 본 연구에서는 Fe기지에 서브마이크론 크기의 미세한 TiC 입자가 균일하게 분산된 Fe-TiC 복합분말을 경제적으로 제조하기 위해 순수한 Fe, Ti 원료분말에 비해 단가가 낮고 미세 분쇄가 용이한 FeO, $TiH_2$ 분말을 고에너지 밀링 후 반응 열처리 시키는 유사 기계화학적 공정을 시도하였다. 조성비 Fe-30wt%TiC 복합분말을 제조하기위해 마이크론(micron) 크기의 FeO, $TiH_2$, C 분말을 사용하였고, 1단계로 FeO와 C을 고에너지 밀링으로 혼합 후 반응시켜 환원시키는 공정과 2단계로 이렇게 환원된 분말과 TiH2를 고에너지 밀링으로 다시 혼합, 분쇄한 후 반응열처리 하는 두 단계 공정을 사용하였다. FeO의 환원 단계에서는 $700{\sim}1,000^{\circ}C$ 온도 범위에서 1시간 유지하였고, 고에너지 밀링 시 밀링시간, 회전속도를 변수로 두고 실험하였다. 환원된 분말은 수평관상로를 이용해 아르곤분위기에서 $1,000{\sim}1300^{\circ}C$까지 1시간 유지하여 반응열처리시켜 Fe-TiC 복합분말을 제조하였다. 준비된 복합분말을 XRD와 FE-SEM, EDS, 입도분석기 (LPSA) 등을 이용해 분말의 형태와 특성, 상, 조성, 입도, 분산도 등을 조사하였다. 제조된 Fe-TiC 나노복합분말을 방전플라즈마소결(SPS) 과 상압소결 실험을 진행하였다. Fe-TiC 복합분말 제조공정의 첫 번째 단계인 FeO의 환원반응은 $800^{\circ}C$이상의 온도에서 Fe로 환원이 진행됨을 확인하였다. 두 번째 단계인 반응열처리공정에서는 $1,000^{\circ}C$ 이상에서 TiC가 형성됨을 XRD 상분석을 통해 확인할 수 있었고, $1,100^{\circ}C$ 이상의 온도에서 반응열처리를 했을 때 XRD 분석결과와 산소 조성 분석 결과로부터 반응의 완결성과 순도에서 최적 온도 조건임을 확인하였다. 온도를 $1,300^{\circ}C$로 증가시킬 경우 반응의 완결성에 큰 변화가 없는 반면 분말입자간의 목형성이 일어나 가소결 되는 것을 FE-SEM을 통해 관찰하였다. 또한 최적조건으로 제조된 Fe-TiC 복합분말의 입도분석과 FE-SEM/EDS 관찰/분석을 시행한 결과 평균 입도 0.6 ${\mu}m$의 미세한 Fe-TiC 복합분말 내에 Fe분말 주변과 내부에 나노크기의 TiC입자가 균일하게 분산되어 존재하는 것을 확인하였다.

• Clean Technology
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• v.16 no.3
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• pp.191-197
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• 2010

Repair reaction of plasma damaged porous methyl doped SiOCH films was carried out with silylation agents dissolved in supercritical carbon dioxide ($scCO_2$) at various reaction time, pressure, and temperature. While a decrease in the characteristic bands at $3150{\sim}3560cm^{-1}$ was detectable, the difference of methyl peaks was not identified apparently in the FT-IR spectra. The surface hydrophobicity was rapidly recovered by the silylation. In order to induce effective repair in bulk phase, the wafer was heat treated before reaction under vacuum or ambient condition. The contact angle was slightly increased after the treatment and completely recovered after the subsequent silylation. Methyl groups were decreased after the plasma damage, but their recovery was not identified apparently from the FT-IR, spectroscopic ellipsometry, and secondary ion mass spectroscopy analyses. Furthermore, Ti evaporator was performed in a vacuum chamber to evaluate the pore sealing effect. The GDS analysis revealed that the open pores in the plasma damaged films were efficiently sealed with the silylation in $scCO_2$.

• Korean Journal of Materials Research
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• v.3 no.1
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• pp.12-18
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• 1993

Abstract The effect of the film stress on the thermal stability of TiSi, films under the dielectric overcoat was investigated. TiS$i_2$ films with the sheet resistance of 1.2 ohm/sq. were produced by a solid-state reaction between sputtered Ti film and single-crystalline Si in an RTA (rapid thermal anneal) machine. Dielectric overcoats such as the USG (Undoped Silicate Glass, Si$O_2$) film and the PE-SiN(S$i_3$$N_4$) film were deposited by AP-CVD and PE-CVD, respectively, on the TiS$i_2$ film. The thermal stability of the TiSi, film was evaluated by changes in the sheet resistance, film stress and microstructure after furnace anneals at 90$0^{\circ}C$. Agglomeration of the TiSi2 film high temperatures results in the increase of sheet resistance and the decrease of tensile stress of TiSi, film. The stress level of the TiSi" PE-SiN and ~SG films at 90$0^{\circ}C$C was 1.3${\times}{10^{9}}$, 1.25 ${\times}{10^{10}}$, 2.26 ${\times}{10^{10}}$ dyne/c$m^2$ in tensile, respectively. Dielectric films deposited by CVD on TiSi, was effective on preventing agglomeration of TiSi,. The PE-SiN film mproved the thermal stability of TiSi, more effectively than the AP-CVD USG film. It is considered that agglomeration of the TiS$i_2$ film under the stress of dielectric overcoat at high temperature can be caused by a diffusional flow of atom called Nabarro-Herring microcreep.reep.

• Polymer(Korea)
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• v.33 no.4
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• pp.290-296
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• 2009

The morphology and mechanical properties of epoxy/polyamide/MPD/2E4MZ-CN reactive blends with various amount of catalyst were investigated. The cure behaviors, mechanical strengths, and morphological changes of the epoxy blend systems were analyzed by using DSC, UTM, and SEM, respectively. The amount of catalyst ranged from 0 to 3 phr, and the cure reaction occurred at $170^{\circ}C$ for 30 min. The maximum peaks in heat flow during cure reactions appeared at slightly lower temperature with increasing catalyst content, indicating that the cure reactions start at lower temperature by adding catalyst and polyamide rarely hinders the cure reaction paths. The co-continuous morphology was found in epoxy/polyamide(20 phr) blends and by adding catalyst to the blends much clearer and uniform co-continuous phase was observed. The surface tension of the mechanical test specimen was increased due to the AP plasma surface treatment, and then adhesion strength was increased by over 20% by adding 2 phr of catalyst to the blends. When considering morphological tuning of the blends by means of catalyst incorporation, it is expected that the increased elongation and adhesion strength can be achieved in the structural adhesive systems.

• Applied Chemistry for Engineering
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• v.25 no.1
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• pp.41-46
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• 2014

The property improvement of polycarbonate coated with a multilayer film composed of an inorganic $SiO_2$ film and a photocatalytic $TiO_2$ film was studied. The $SiO_2$ film as a binder had an excellent light transmission characteristic. After the treatment with atmospheric pressure plasma, the surface of $SiO_2$ film showed the hydrophilicity, which increased the film coating uniformity with a $TiO_2$-containing aqueous solution. When $TiO_2$ film was over 200 nm thick, the absorption effect of UV rays in the range of 180~400 nm suppressed the yellowing phenomena of polycarbonate substrate. The inorganic film improved the heat resistance of polycarbonate substrates. $TiO_2$ film in the outmost under the exposure of UV rays promotes the catalytic oxidation characteristics and yields the capability to the decomposition of organic contaminants, and also increases the self-cleaning properties due to the increase of hydrophilicity. Structural stability of the polycarbonate substrate coated with inorganic $TiO_2$ and $SiO_2$ film was shown. The role of $SiO_2$ film between $TiO_2$ and polycarbonate substrate suppressed the peeling of $TiO_2$ film by inhibiting the photocatalytic oxidation effect of $TiO_2$ film on the polycarbonate substrate.

• Korean Journal of Soil Science and Fertilizer
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• v.42 no.5
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• pp.399-407
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• 2009

Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.