• Journal of Powder Materials
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• v.22 no.6
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• pp.426-431
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• 2015

Microstructural examination of the Nb-Si-B alloys at Nb-rich compositions is performed. The Nb-rich corner of the Nb-Si-B system is favorable in that the constituent phases are Nb (ductile and tough phase with high melting temperature) and $T_2$ phase (very hard intermetallic compound with favorable oxidation resistance) which are good combination for high temperature structural materials. The samples containing compositions near Nb-rich corner of the Nb-Si-B ternary system are prepared by spark plasma sintering (SPS) process using $T_2$ and Nb powders. $T_2$ bulk phase is made in arc furnace by melting the Nb slug and the Si-B powder compact. The $T_2$ bulk phase was subsequently ball-milled to powders. SPS is performed at $1300^{\circ}C$ and $1400^{\circ}C$, depending on the composition, under 30 MPa for 600s, to produce disc-shaped specimen with 15 mm in diameter and 3 mm high. Hardness tests (Rockwell A-scale and micro Vickers) are carried out to estimate the mechanical property.

• Journal of the Korean Society for Heat Treatment
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• v.17 no.1
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• pp.17-22
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• 2004

In the present study, newly developed spark plasma sintering(SPS) technique was introduced to refine the grain size of ${\gamma}$-based TiAl intermetallic compounds. Ti-46Al-1.5Mo and Ti-46Al-1.5Mo-0.2C(at%) prealloyed powders were produced by mechanical milling(MM) in high-energy attritor. The mechanically milled powders were characterized by XRD and SEM for the microstructural evolution as a function of milling time. And then, the MMed powders were sintered by both spark plasma sintering and hot pressing in vacuum (HP). After the sintering process, MM-SPSed specimens were heat-treated in a vacuum furnace (SPS-VHT) and in the SPS equipment(MM-SPS) for microstructural control. It was found from microstrutural observation that the microstructure consisting of equiaxed ${\gamma}$-TiAl with a few hundred nanometer in average size and ${\alpha}_2-Ti_3Al$ particles were formed after both sintering processes. It was also revealed from hardness test and three-point bending test that the effect of grain refinement on the hardness and bending strength is much higher than that of carbon addition. The fully lamellar microstructures, which is less than $80{\mu}m$ in average grain size was obtained by SPS-VHT process, and the fully lamellar microstructure which is less than $100{\mu}m$ in average grain size was obtained by MM-SPS for a relatively shorter heat-treatment time.

• Journal of Korea Foundry Society
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• v.19 no.6
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• pp.493-500
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• 1999

Squeeze casting was used for fabricating a light metal base composite having high strength and wearresistance. Reactive sintering was used to prepare the preform of Squeeze casting. To utilize Fe-Al intermetallic compounds and SiC particle as a reinforcement, there needs to prepare Fe-Al mixed powder at 50, 60, 70at.%Al, and add SiC powder to the above mixture at 4, 7, 16, 24wt.%. The prepared mixture with SiC was reactive sintered in a tube furnace at $660^{\circ}C$ to get a porous hybrid preform of intermetallic compound and SiC. The preform prepared above was placed in a metal mold, preheated at $660^{\circ}C$ AC4C matrix was injected into the mold with the temperature of the melt at $610^{\circ}C$ After these processes, 66MPa was applied to the mold for 5 minute to finish the whole procedure. The maximum reaction temperature was increased with the increased Al amount, but decreased with the increased SiC amount. The density of the preform was decreased with SiC amount increase in the compacts due to swelling of the preform. An optical microscope was applied to observe the micro structure and the dispersion of the reinforcements. To analyze phases, We utilized XRD, EDS. Hardness test were chosen to get the information of mechanical properties. There were no significant changes in micro structure between the composite and preform. However, it was shown that uniform dispersion of the reinforcers and complete infiltration of the melt into the preform were achieved through the procedure of the squeeze casting. It was observed that the hardness of the composite is decreased with increased SiC amount, resulting from the volumetric expansion of the preform.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 1995.11a
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• pp.25-25
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• 1995

Liquid phase sintering of 90W-6Ni-4Mn alloy has been investigated as functions of sintering atmosphere, heating rate, and reduction temperature. The present work accounts for the thermodynamic oxidatiodreduction reactions of constituent powders of W, Ni and Mn. By discounting these reactions, the previous investigations would obtain only the alloy with large pores and the lowered relative sintered density, by the liquid phase sintering under a dry hydrogen atmosphere. the sintering cycle consisted of a rapid heating to reduction temperatures under high purity nitrogen atmosphere, and holding for 4 hours and sintering at $1260^{\circ}C$ for 1 hour under a dry hydrogen gas. The relative density of the sintered alloy increased with increasing heating rate. As the reduction temperature increased, the relative density increased to the lm theotical density at the duction temture above $1150^{\circ}C$. The mimsturcatre of sintered alloys has been analysed by a scanning election microscope. The sintered density was compared with those obtained from the other investigators. It was found that the reduction $1150^{\circ}C$ results in the lowered densification of 90W-6Ni-4Mn alloy. This is caused by the fact that reducing reactions of W and Ni oxides contained in W an Ni powders concomitantly leads to oxidizing reaction of Mn powder the oxidized Mn is hardly reduced at sintering temperature and thereby remains large pores in the alloy. It is concluded that the W-Ni-Mn alloy with full density can be obtained by the precise control of atmosphere, heating rate, and sintering temperature.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.236-236
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• 2010

알루미늄 자체에 대한 질화 기술의 어려움 때문에 현재까지는 AlN 분말을 이용한 소결 공정을 통하여 주요 부품의 제작이 되어 왔으며. Al 질화 기술보다는 아노다이징과 같은 표면 산화 공정 또는 도금과 같은 기술이 선호되어 왔다. 알루미늄 질화 기술이 잘 사용되지 않았던 이유는 알루미늄 표면에 2 5 nm 두께로 존재하는 치밀한 산화층의 높은 안정성 때문에 질화반응이 어렵기 때문이다. 이 알루미늄 산화물의 안정성은 질화물에 비교하여 5 배까지 높으며, 이런 경향은 온도가 높아짐에 따라 더욱 커지기 때문이다. 특히, 알루미늄의 낮은 기계적 물성을 향상시키기 위해서는 충분히 깊은 두께로 형성되어야 할 필요성이 높으나 알루미늄에 대한 질소의 고용도가 거의 없고 확산 계수가 매우 낮기 때문에 충분히 두꺼운 질화층의 형성이 어렵기 때문이다. 결국, 알루미늄 질화가 가능하기 위해서는 표면의 산화층을 없애야 하며, 알루미늄이 AlN이 되려는 속도는 $Al_2O_3$를 만드려는 속도보다 매우 느리므로, 잔존 산소량을 최소화 할 필요성이 있어서 고진공 분위기에서 처리되어야 한다. 일반적으로 알루미늄 질화를 위해서는 $10^{-6}\;torr$ 이하의 고진공도의 챔버가 필요하며 고순도의 반응 가스를 사용하여야 한다. 그러나 이러한 고진공하에서는 낮은 이온밀도 때문에 신속질화가 기존의 공정시간인 20시간동안, AlN층이 5um이하로 형성되었다. 본 연구에서, 알루미늄의 질화에 있어서, 표면층에 높은 전류를 걸어주어, 용융상태로 만들어주는 것이 좋다는 연구 결과를 얻었으며, 이를 토대로 신속질화를 위하여 전류밀도(전력량)에 따라 알루미늄 질화층의 형성 정도를 연구하였다. SEM, EDS, XRD등을 통해 Al의 표면에 플라즈마 질화를 통해 Al에 질소의 함유량이 증가하는 것을 확인하였으며 광학현미경을 통해 질화층의 두께와 표면조직을 확인하였다. Al 시편의 표면을 효과적으로 활성화할 수 있는 $400^{\circ}C$ 이상의 온도에서 전류밀도(전력량)와 시간의 변화에 따라 질화층이 효과적으로 형성되는 조건과 시간에 따라 두께가 증가하는 경향을 확인할 수 있었다. 이러한 신속 질화 공정을 통해 2시간 이내의 질화를 통해 40um이상의 AlN층을 형성할 수 있었다.

• Korean Journal of Materials Research
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• v.15 no.7
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• pp.439-443
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• 2005

The oxidation behavior and the thermal stability of nanocrystalline Al-25Ti-8Mn intermetallic compound were investigated. $Al_3Ti$ intermetallic compound, which has a potential for high temperature structural material, was fabricated by mechanical alloying(MA) with $8at.\%$ Mn to enhance the thermal stability and ductility. And Al-25Ti-8Mn intermetallic compound was sintered by spark plasma sintering(SPS) at $700^{\circ}C$. After sintering process, cubic $Ll_2$ structure was maintained without phase transformation and the grain size was about 50nm. To investigate the oxidation behavior of the specimens, thermal gravimetric analysis(TGA) was performed at 700, 800, 900, and $1000^{\circ}C$ for 24 h in $O_2$. As the temperature increased from $700^{\circ}C\;to\;900^{\circ}C$ the weight gain of specimens increased. However at $1000^{\circ}C$, unlike the oxidation behavior of $700^{\circ}C\;to\;900^{\circ}C$, the weight gain of specimen decreased drastically and the transition from linear rate region to parabolic rate region occurred rapidly due to the dense $\alpha-Al_2O_3$.

• Journal of Powder Materials
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• v.28 no.4
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• pp.336-341
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• 2021

In this study, a nanocrystalline FeNiCrMoMnSiC alloy was fabricated, and its austenite stability, microstructure, and mechanical properties were investigated. A sintered FeNiCrMoMnSiC alloy sample with nanosized crystal was obtained by high-energy ball milling and spark plasma sintering. The sintering behavior was investigated by measuring the displacement according to the temperature of the sintered body. Through microstructural analysis, it was confirmed that a compact sintered body with few pores was produced, and cementite was formed. The stability of the austenite phase in the sintered samples was evaluated by X-ray diffraction analysis and electron backscatter diffraction. Results revealed a measured value of 51.6% and that the alloy had seven times more austenite stability than AISI 4340 wrought steel. The hardness of the sintered alloy was 60.4 HRC, which was up to 2.4 times higher than that of wrought steel.

• Journal of Powder Materials
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• v.28 no.3
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• pp.221-226
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• 2021

We fabricate the non-equiatomic high-entropy alloy (NE-HEA) Fe_49.5Mn₃₀Co₁₀Cr₁₀C_0.5 (at.%) using spark plasma sintering under various sintering conditions. Each elemental pure powder is milled by high-energy ball milling to prepare NE-HEA powder. The microstructure and mechanical properties of the sintered samples are investigated using various methods. We use the X-ray diffraction (XRD) method to investigate the microstructural characteristics. Quantitative phase analysis is performed by direct comparison of the XRD results. A tensile test is used to compare the mechanical properties of small samples. Next, electron backscatter diffraction analysis is performed to analyze the phase fraction, and the results are compared to those of XRD analysis. By combining different sintering durations and temperature conditions, we attempt to identify suitable spark plasma sintering conditions that yield mechanical properties comparable with previously reported values. The samples sintered at 900 and 1000℃ with no holding time have a tensile strength of over 1000 MPa.

• Journal of Powder Materials
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• v.29 no.5
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• pp.399-410
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• 2022

Changes in the mechanical properties and microstructure of an IN 939 W alloy according to the sintering heating rate were evaluated. IN 939 W alloy samples were fabricated by spark plasma sintering. The phase fraction, number density, and mean radius of the IN 939 W alloy were calculated using a thermodynamic calculation. A universal testing machine and micro-Vickers hardness tester were employed to confirm the mechanical properties of the IN 939 W alloy. X-ray diffraction, optical microscopy, field-emission scanning electron microscopy, Cs-corrected-field emission transmission electron microscopy, and energy dispersive X-ray spectrometry were used to evaluate the microstructure of the alloy. The rapid sintering heating rate resulted in a slightly dispersed γ' phase and chromium oxide. It also suppressed the precipitation of the η phase. These helped to reinforce the mechanical properties.

• Journal of Powder Materials
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• v.30 no.6
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• pp.484-492
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• 2023

In this study, Ni-Y₂O₃ powder was prepared by alloying recomposition oxidation sintering (AROS), solution combustion synthesis (SCS), and conventional mechanical alloying (MA). The microstructure and mechanical properties of the alloys were investigated by spark plasma sintering (SPS). Among the Ni-Y₂O₃ powders synthesized by the three methods, the AROS powder had approximately 5 nm of Y₂O₃ crystals uniformly distributed within the Ni particles, whereas the SCS powder contained a mixture of Ni and Y₂O₃ nanoparticles, and the MA powder formed small Y₂O₃ crystals on the surface of large Ni particles by milling the mixture of Ni and Y₂O₃. The average grain size of Y₂O₃ in the sintered alloys was approximately 15 nm, with the AROS sinter having the smallest, followed by the SCS sinter at 18 nm, and the MA sinter at 22 nm. The yield strength (YS) of the SCS- and MA-sintered alloys were 1511 and 1688 MPa, respectively, which are lower than the YS value of 1697 MPa for the AROS-sintered alloys. The AROS alloy exhibited improved strength compared to the alloys fabricated by SCS and conventional MA methods, primarily because of the increased strengthening from the finer Y₂O₃ particles and Ni grains.