• 한국표면공학회지
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• 제37권2호
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• pp.80-85
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• 2004

Chromium-carbon (Cr-C) and chromium-carbon-phosphorus (Cr-C-P) alloy deposits using trivalent chromium sulfate baths containing potassium formate were prepared to study their current efficiency, hardness change and phase transformations behavior with heat treatment, respectively. The current efficiencies of Cr-C and Cr-C-P alloy deposits increase with increasing current density in the range of 15-35 A/dm$^2$. Carbon content of Cr-C and phosphorous of Cr-C-P layers decreases with increasing current density, whereas, the carbon content of Cr-C-P layer is almost constant with the current density. Cr-C deposit shows crystallization at $400^{\circ}C$ and has (Cr+Cr$_{ 23}$$C_{6}$) phases at $800^{\circ}C$. Cr-C-P deposit shows crystallization at $600^{\circ}C$ and has (Cr+Cr$_{23}$ $C_{6}$$+Cr_3$P) phases at $800^{\circ}C$. The hardness of Cr-C and Cr-C-P deposits after heating treatment for one hour increase up to Hv 1640 and Hv 1540 and decrease about Hv 820 and Hv 1270 with increasing annealing temperature in the range of $400～^{\circ}C$, respectively. The hardness change with annealing is due to the order of occurring of chromium crystallization, precipitation hardening effect, softening and grain growth with temperature. Less decrease of hardness of Cr-C-P deposit after annealing above $700^{\circ}C$ is related to continuous precipitation of $Cr_{23}$ $C_{6}$ and $Cr_3$P phases which retard grain growth at the temperature.

• Metals and materials international
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• 제24권6호
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• pp.1193-1201
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• 2018

Dilatometry is a useful technique to obtain experimental data concerning transformation. In this paper, a dilation conversional model was established to calculate carbides fraction in AISI H13 hot-work tool steel based on the measured length changes. After carbides precipitation, the alloy contents in the matrix changed. In the usual models, the content of carbon atoms after precipitation is considered as the only element that affects the lattice constant and the content of the alloy elements such as Cr, Mo, Mn, V are often ignored. In the model introduced in this paper, the alloying elements (Cr, Mo, Mn, V) changes caused by carbides precipitation are incorporated. The carbides were identified using scanning electron microscope and transmission electron microscope. The relationship between lattice constant of carbides and temperature are measured by high-temperature X-ray diffraction. The results indicate that the carbides observed in all specimens cooled at different rates are V-rich MC and Cr-rich $M_{23}C_6$, and most of them are V-rich MC, only very few are Cr-rich $M_{23}C_6$. The model including the effects of substitutional alloying elements shows a good improvement on carbides fraction predictions. In addition, lower cooling rate advances the carbides precipitation for AISI H13 specimens. The results between experiments and mathematical model agree well.

• 대한금속재료학회지
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• 제49권2호
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• pp.93-103
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• 2011

Precipitation behavior of high-nitrogen duplex Fe-24Cr-7Mn-4Ni-4Mo-0.43N stainless steel aged at $850^{\circ}C$ was investigated using scanning transmission electron microscopy. Based on the analyses of selected area diffraction patterns, four kinds of precipitates (intermetallic sigma (${\sigma}$) and chi (${\chi}$), $Cr_2N$ and secondary austenite) were identified. At the ferrite/austenite phase boundary, the ${\sigma}$ phase and secondary austenite were formed via ${\alpha}{\rightarrow}{\gamma}+{\sigma}$ eutectoid reaction. The precipitation of $Cr_2N$ occurred at the austenite grain boundary as well as the interior of the ferrite. The intermetallic ${\chi}$ phase also formed within the ferrite and showed a cube-cube orientation relationship with the ferrite. Further aging produced a lamellar structure composed of $Cr_2N$ and austenite along the ferrite/austenite boundary and enhanced the precipitation of the ${\chi}$ phase. The crystallographic features of the precipitates were also examined in terms of the orientation relationship with the austenite or ferrite matrix.

• 열처리공학회지
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• 제11권3호
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• pp.192-199
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• 1998

This study was carried out to investigate the influence of variations in the temperature and time of isothermal heat treatment, applied stresses and prestrain on the isothermal transformation behavior of ${\gamma}$ and ${\sigma}$ phases and mechanical properties of 25Cr-7Ni-3Mo duplex stainless steel. The precipitation of ${\gamma}$ and ${\sigma}$ phases through isothermal heat treatment showed the type curves with a certain incubation period, the curve migrated to in a short period of time and the amount of precipitation increased with decreasing isothermal heat treatment temperature. Under the state of isothermal transformation, the precipitation of ${\gamma}$ and ${\sigma}$ phases was stimulated by applied stress, with increasing applied stress, the curves migrated to in a short period of time and also observed that the application of stress has a greater influence on the amount of ${\sigma}$ precipitation than that of ${\gamma}$ precipitation. The precipitation of ${\gamma}$ and ${\sigma}$ phases was stimulated by cold and warm rolling before isothermal heat treatment and precipitation of ${\gamma}$ and ${\sigma}$ phases has a greater influence on the warm rolling than cold rolling. The tensile strength and hardness increased with increasing cold and warm rooling reduction ratio.

• 한국결정성장학회지
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• 제17권6호
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• pp.264-271
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• 2007

본 연구에서는 $Fe_2O_3-CoO-Cr_2O_3-MnO_2$계 색상의 무기안료를 공침법을 사용하여 합성하였다. 출발원료로는 $FeCl_3,\;CoCl_2,\;CrCl_3,\;MnCl_2$를 사용하였으며 침전제로는 2N-KOH를 사용하였다. $MnCl_2$는 10 mole%로 고정한 후 세 가지 원료로서 6가지 조성비를 만들어 안료를 합성하였다. 조합된 시료는 1.5시간 $1350^{\circ}C$에서 하소하였다. XRD, FT-IR, SEM 과 UV spectrophotometer를 사용하여 안료의 특성 분석을 하였다. 합성된 안료는 석회유, 석회 바륨유에 각각 6wt%씩 첨가하여 $1260^{\circ}C$ 산화소성, $1240^{\circ}C$ 환원 소성하였다. UV Spectrometer를 사용하여 색상분석을 한 결과는 black, bluish black, dark grayish green을 나타냈다.

• 한국재료학회지
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• 제33권2호
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• pp.77-86
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• 2023

High-temperature oxidation of a Ni-based superalloy was analyzed with samples taken from gas turbine blades, where the samples were heat-treated and thermally exposed. The effect of Cr/Ti/Al elements in the alloy on high temperature oxidation was investigated using an optical microscope, SEM/EDS, and TEM. A high-Cr/high-Ti oxide layer was formed on the blade surface under the heat-treated state considered to be the initial stage of high-temperature oxidation. In addition, a PFZ (γ' precipitate free zone) accompanied by Cr carbide of Cr₂₃C₆ and high Cr-Co phase as a kind of TCP precipitation was formed under the surface layer. Pits of several ㎛ depth containing high-Al content oxide was observed at the boundary between the oxide layer and PFZ. However, high temperature oxidation formed on the thermally exposed blade surface consisted of the following steps: ① Ti-oxide formation in the center of the oxide layer, ② Cr-oxide formation surrounding the inner oxide layer, and ③ Al-oxide formation in the pits directly under the Cr oxide layer. It is estimated that the Cr content of Ni-based superalloys improves the oxidation resistance of the alloy by forming dense oxide layer, but produced the σ or µ phase of TCP precipitation with the high-Cr component resulting in material brittleness.

• Applied Biological Chemistry
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• 제41권1호
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• pp.89-94
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• 1998

크롬의 산화는 자연계에 존재하는 여러 가지의 Mn-oxide에 의해 일어나며 산화과정에 존재하는 크롬 화학종들은 반응계 내에서 흡착, 침전 현상을 유발할 수 있고 결과적으로 산화반응을 조절할 수 있을 것이다. 본 연구에서는 birnessite와 pyrolusite에 의한 크롬의 산화에서 크롬 화학종이 반응에 미치는 영향을 조사하였다 Mn-oxide는 그 종류에 따라 크롬 산화력에서 큰 차이를 보였으며 용액의 pH와 초기 3가 크롬 첨가량도 산화반응에 큰 영향을 미쳤다. 동일 표면적당의 산화력을 비교하면 pyrolusite의 산화력은 birnessite의 5% 정도에 불과하였다. 이는 pyrolusite 의 결정도에 크게 기인하며 또한 양으로 하전된 표면 특성 때문에 반응물인 3가 크롬의 접근이 어렵고 반응산물인 6가 크롬의 흡착 등에 기인하는 것으로 보인다. Birnessite에 의한 산화반응에서 pH 3에서는 oxide의 표면에서의 크롬 화학종들의 흡착이나 침전 현상은 발견되지 않았으며 pyrolusite의 경우 일부 6가 크롬의 흡착이 나타났으나 침전현상은 발견되지 않았다. 따라서 pH 3의 경우 산화반응은 Mn-oxide의 특성에 따라 결정된다. Mn-oxide에 의한 크롬의 산화는 열역학적으로 용액의 pH가 높아질수록 더 진행되어야 한다. Birnessite의 경우 pH 5에서 오히려 산화반응이 현저히 저해되었는데 이는 birnessite의 표면에 형성되는 3가 크롬의 침전이 반응표면을 감소시킴으로써 나타나는 현상으로 판단된다. Pyrolusite의 경우 pH 3보다 pH 5에서 크롬의 산화는 더 일어나나 초기 3가 크롬의 첨가량이 많아지면서 반응이 억제된다. 일부 3가와 6가 크롬의 흡착이 일어나나 이 경우도 역시 pyrolusite의 표면에 형성되는 3가 크롬의 침전이 반응을 조절하는 주 요인으로 생각된다. Mn-oxide의 표면에 형성되는 3가 크롬의 침전은 산화가 일어날 수 있는 반응표면을 감소시키고 또한 반응물의 농도를 낮춤으로써 용액의 pH가 높고 3가 크롬의 첨가량이 많아질 때 크롬의 산화반응을 억제하는 주 요인이 되는 것으로 판단된다.

• 한국분말재료학회지
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• 제13권3호
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• pp.178-186
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• 2006

The effect of use of $H_2O$ as PCA(process control agent) to prevent the carbon contamination during mechanical alloying process and the precipitation behavior in Ni-20Cr-20Fe-5Nb bulk alloy after aging were investigated. NbC and $Cr_2O_3$ were formed during mechanical alloying and consolidation processes in the Ni-20Cr-20Fe-5Nb alloy in which methanol($CH_3OH$) was added as PCA. Formation of NbC in this alloy decreased the amount of Nb dissolved in the Ni matrix. The use of $H_2O$ as PCA in Ni-20Cr-20Fe-5Nb alloy prevented the formation of NbC and increased the hardness. The increase of hardness in this alloy was attributed to the increased amount of Nb dissolved in the Ni matrix. After aging treatment for 20 hours at $600^{\circ}C\;and\;720^{\circ}C$ of Ni-20Cr-20Fe-5Nb bulk alloy in which $H_2O$ added as PCA, ${\gamma}"$$(Ni_3Nb,\;tetragonal)\;and\;{\delta}\;(Ni_3Nb,\;orthorhombic)$ precipitates were formed, respectively. The precipitation temperatures of ${\gamma}"$ and ${\delta}$ in this bulk alloy were lower than those in commercial IN 718 alloy. It seemed that the lower precipitation temperatures for ${\gamma}"$ and ${\delta}$ in this bulk alloy than in commercial IN 718 alloy were due to severe plastic deformation during mechanical alloying.

• 열처리공학회지
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• 제9권3호
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• pp.205-211
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• 1996

Structural studies have been performed on precipitation hardening discovered in $Ll_2$-ordered $Ni_3$(Al,Cr) containing 0.2 and 0.5 mol% of carbon in terms of transmission electron microscopy(TEM). By aging at temperatures around 1073 K after solution treatment at 1423 K, fine polyhedral precipitates appear firstly on the dislocations and then in the matrix. The selected area electron diffraction (SAED) studies revealed that these particles are a $M_{23}C_6$ type carbide which has the cube-cube orientation relationship with the matrix lattice. Weak-beam electron microscopy observations of deformation induced dislocations suggested that the dislocations bypass the carbide particles during deformation.

• 한국재료학회:학술대회논문집
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• 한국재료학회 1996년도 재료학회 추계학술발표회
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• pp.23-23
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• 1996