• Journal of Powder Materials
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• v.19 no.1
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• pp.32-39
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• 2012

This study investigated refinement behaviors of TiC powders produced under different impact energy conditions using a mechanical milling process. The initial coarse TiC powders with an average diameter of 9.3 ${\mu}m$ were milled for 5, 20, 60 and 120 mins through the conventional low energy mechanical milling (LEMM, 22G) and specially designed high energy mechanical milling (HEMM, 65G). TiC powders with angular shape became spherical one and their sizes decreased as the milling time increased, irrespective of milling energy. Based upon the FE-SEM and BET results of milled powders, it was found initial coarse TiC powders readily became much finer near 100 nm within 60 min under HEMM, while their sizes were over 200 nm under LEMM, despite the long milling time of up to 120 min. Particularly, ultra-fine TiC powders with an average diameter of 77 nm were fabricated within 60 min in the presence of toluene under HEMM.

• Korean Journal of Metals and Materials
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• v.49 no.2
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• pp.161-166
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• 2011

The aim of this study was to determine the effect of high-energy mechanical milling (HEMM) time and sintering temperature on microstructure and mechanical properties of the TiAl composite fabricated by pulse current activated sintering. TiAl intermetallic powders were milled by HEMM for 1h, 4h, and 8h respectively. Thermal analysis was used to observe the phase transformation of the milled TiAl powders. The sintering time decreased with increase of milling time. The hardness and fracture toughness of the sintered specimens also was improved with increasing milling time. The grain size of the sintered specimens which was milled for 4h was in the range of 50~100 nm.

• Korean Journal of Materials Research
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• v.17 no.11
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• pp.587-592
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• 2007

Al-42wt%Nb powder was prepared by high-energy mechanical milling(HEMM). The particle size, phase transformation and microstructure of the as-milled powder were investigated by particle size distribution (PSD) analyzer, scanning electron microscopy (SEM), X-ray diffractometery (XRD), transmission electron microscopy (TEM)and differential thermal analysis (DTA). The milled powders were heated to a sintering temperature at 1000C with under vaccum with vaccum tube furnace. Microstructural examination of sintered Ti-42wt%Nb alloy using 4h-milled powder showed Ti-rich phases (${\alpha}$-Ti) which are fine and homogeneously distributed in the matrix (Nb-rich phase: ${\beta}$-Ti). The sintered Ti-42wt%Nb alloy with milled powder showed higher hardness. The microstructure of the as quenched specimens fabricated by sintering using mixed and milled powder almost are same, but the hardness of as quenched specimen fabricated by using mixed powder increased due to solution hardening of Nb in Ti matrix. The aging effect of these specimens on microstructural change and hardening is not prominent.

• Korean Journal of Metals and Materials
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• v.50 no.6
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• pp.469-475
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• 2012

A high-energy mechanical milling (HEMM) process was introduced to improve sinter-ability, and rapid sintering of spark plasma sintering (SPS) under pressure was used to make ultra fine grain (UFG) of Ti-Nb-Mo-CPP composites, which have bio-attractive elements, for increasing mechanical properties. Ti-Nb-Mo-CPP composites were successfully fabricated by SPS at $1000^{\circ}C$ within 5 minutes under 70 MPa using HEMMed powders. The Vickers hardness of the composites increased with increased milling time and addition of CPP contents. Biocompatibility and corrosion resistance of the Ti-Nb-Mo alloys were improved by addition of CPP, and the Ti-35%Nb-10%Mo-10%CPP alloy had better biocompatibility and corrosion resistance than the Ti-6Al-4V ELI alloy.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.05a
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• pp.48.2-48.2
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• 2009

Ti와 Ti-6%Al-4%V합금은 내 부식성 및 생체 적합성이 매우 우수하기 때문에 현재 생체재료로써 널리 사용되고 있다. 하지만 Ti-6%Al-4V합금에 포함된 Al과 V이 신체에 좋지 않은 영향을 줄 수 있다는 연구 결과가 보고되면서 새로운 생체재료의 연구가 활발히 진행되고 있다. 본 연구에서는 생체에 무해한 Ti-Nb와 hydroxyapatite(HAp)를 복합 첨가하여 고에너지볼밀링(high-energy mechanical milling, HEMM)으로 나노 합금분말을 제조 후 급속소결에 의하여 Ti-Nb/HAp 생체재료를 제조 하였다. 제조한 Ti-Nb/HAp 생체용 복합재료에서 HAp 첨가량과 분말의 밀링, 믹싱에 따른 조직 변화와 소결체의 생체적합성의 변화 및 기계적 특성의 변화를 분석하였다. 이때 Ti-42%Nb에 HAp의 첨가량을 0%, 5%, 10%, 15%로 변화를 주었고, 밀링은 고에너지볼밀링기를 이용하여 0~8시간 동안 실시하였다. 그 결과 밀링 시간이 증가할수록 합금 분말의 크기가 미세해졌으며, 특히 8시간 밀링시 분말의 크기가 나노 크기로 감소하여 기계적 특성(경도 및 강도)이 우수해지는 것을 알 수 있었다.

• Journal of Powder Materials
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• v.17 no.6
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• pp.443-448
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• 2010

The $\beta$ phase Ti-Nb-Sn-HA bio materials were successfully fabricated by high energy mechanical milling and pulse current activated sintering (PCAS). Ti-6Al-4V ELI alloy has been widely used as biomaterial. But the Al has been inducing Alzheimer disease and V is classified as toxic element. In this study, ultra fine sized Ti-Nb-Sn-HA powder was produced by high energy mechanical milling machine. The $\beta$ phase Ti-Nb-Sn-HA powders were obtained after 12hr milling from $\alpha$ phase. And ultra fine grain sized Ti-Nb-Sn-HA composites could be fabricated using PCAS without grain growth. After sintering, the microstructures and phase-transformation of Ti-Nb-Sn-HA biomaterials were analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). The relative density was obtained by Archimedes principle and the hardness was measured by Vickers hardness tester. The $\beta$-Ti phase was obtained after 12h milling. As result of hardness and relative density, 12h milled Ti-Nb-Sn-HA composite has the highest values.

• Korean Journal of Materials Research
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• v.23 no.2
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• pp.135-142
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• 2013

The Ti-6Al-4V extra low interstitial (ELI) alloy has been widely used as an orthopedic implant material because of its excellent mechanical properties and biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity of the Al and V elements. Therefore, non-toxic biomaterials with a low elastic modulus need to be developed. A high energy mechanical milling (HEMM) process is introduced to improve the effect of sintering. Rapid sintering of spark plasma sintering (SPS) under pressure was used to make an ultra fine grain of Ti-25 wt.%Nb-7 wt.%Zr-10 wt.%Mo-(10 wt.%CPP) composites with bio-attractive elements for increasing strength. These composites were fabricated by SPS at $1000^{\circ}C$ at 60 MPa using HEMM powders. During the sintering process, $CaTiO_3$, TixOy, and CaO were formed because of the reaction between Ti and CPP. The effects of CPP content on the physical and mechanical properties of the sintered Ti-Nb-Zr-Mo-CPP composites were investigated. The biocompatibility and corrosion resistance of the Ti-Nb-Zr-Mo alloys were improved by the addition of CPP.

• Korean Journal of Materials Research
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• v.22 no.3
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• pp.150-154
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• 2012

Ti-6Al-4V ELI (Extra Low Interstitial) alloy have been widely used as alternative to bone due to its excellent biocompatibility, although it still has many problems such as high elastic modulus and toxicity. Therefore, biomaterials with low elastic modulus and non toxic characteristics have to be developed. A novel ${\beta}$ Ti-35wt%Nb-7wt%Zr-Calcium pyrophosphate (CPP) composite that is a biocompatible alloy without elemental Al or V was fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70 MPa using high energy mechanical milled (HEMM) powder. The microstructure and phases of the milled powders and the sintered specimens were studied using SEM, TEM, and XRD. Ti-35wt%Nb-7wt%Zr alloy was transformed from ${\alpha}$ phase to ${\beta}$ phase in the 4h-milled powder by sintering. The sintered specimen using the 4h-milled powder showed that all the elements were distributed very homogeneously and had higher density and hardness. ${\beta}$ Ti alloy-CPP composite, which has nanometer particles, was fabricated by SPS using HEMMed powder. During the sintering process, $CaTiO_3$, TixOy, and CaO were formed because of the reaction between Ti and CPP. The Vickers hardness of the composites increases with the increase of the milling time and the addition of CPP. The biocompatibility of the Ti-Nb-Zr alloys was improved by addition of CPP.

• Journal of Powder Materials
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• v.18 no.2
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• pp.188-195
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• 2011

The aim of this study was to investigate microstructures and mechanical properties of nano-sized Ti-35 wt.%Nb-7 wt.%Zr-10 wt.%CPP composite fabricated by high energy mechanical milling (HEMM) and pulse current activated sintering (PCAS). Grain growth of the mechanically milled powder was prevented by performing PCAS. The principal advantages of calcium phosphate materials include: similarity in composition to the bone mineral, bioactivity, osteoconductivity and ability to form a uniquely strong interface with bone. The hardness and wear resistance property of nano-sized Ti-35 wt.%Nb-7 wt.%Zr-10 wt.%CPP composites increased with increasing milling time because of decreased grain-size of sintered composites.