• 한국산업융합학회 논문집
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• 제4권1호
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• pp.27-34
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• 2001

Refining of powder particles and their dissolution into the Al matrix during mechanical alloying(MA) were investigated by using X-ray diffraction(XRD) transmission electron microscopy (TEM) functions of alloy composition, milling time and ball to powder ratio(BPR). It is found that Ti particles less than 20nm are observed in a dark field image of mechanically alloyed Al-10wt%Ti whose XHD pattern exhibits no Ti peak. The observed change of lattice constant of AI indicates that about 1 wt%Ti can he solved in Al after MA for a long time, independent of alloy composition, milling time and BPR, suggesting that most of Ti particles arc retained in the Al matrix. It is concluded that the disappearance of XRD peaks in mechanically alloyed Al-10wt%Ti is not simply attributable to the dissolution of Ti into Al, but associated mainly with extreme refining and/or heavy straining of Ti Particles.

• 한국재료학회지
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• 제11권12호
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• pp.1035-1041
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• 2001

The refining process and solubility of Ti in Al matrix during mechanical alloying (MA) were investigated by using X-ray diffraction (XRD), transmission electron microscopy (TEM) as functions of alloy composition, milling time and ball to powder ratio (BPR). Mechanical alloyed samples were annealed for investigating their stability and the formation behavior of$Al_3Ti$in the temperature range from$200{\circ}C$to$600{\circ}C$. It is observed from present experimental that disappearance of Ti peaks in mechanically alloyed Al-10wt%Ti is not simply attributable to the dissolution of Ti into Al, but associated mainly with extreme refining and/or heavy straining of Ti particles The annealing of the mechanically alloyed Al-Ti powders show differences in aluminide formation behavior when Ti content in Al is equal to or less than l0wt% and higher than l5wt%Ti. When Ti-content in Al is equal to or less than l0wt%, the MA powders transform directly to a global equilibrium state forming $DO_{22}- type\;Al_3$Ti above$400{\circ}C$. In the Al-Ti samples with equal to or higher than l5wt%Ti, transitional phases of cubic$Al_3Ti$and tetragonal $Al_{24}Ti_8$ are formed above$400{\circ}C$. They are stable only below$500{\circ}C$, and, $DO_{22}-type\;Al_3Ti$ becomes dominant aluminide at temperature higher than$ 600{\circ}C$.

• 한국세라믹학회지
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• 제29권5호
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• pp.347-356
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• 1992

Various kaolin samples with different alumina content were prepared from calcined admixture of kaolin and ammonium sulfate by varying the treatment time in sulfuric acid. Samples were nitridated under N2 or N2-H2 atmosphere with changing the amount of added carbon, the reaction time and temperature. As the alumina content lowered, the size of kaolin particles decreased and the specific surface area increased. XRD analysis indicated that ${\alpha}$-quartz remained by decomposition of halloysite and meta-halloysite. Experimental results of nitridation behavior are summerized as follows; 1) Nitridation under N2 atmosphere. With the increase of C/SiO2 ratio and with the decrease of Al2O3 content, disappearance of XRD pattern peaks of mullite, ${\alpha}$-quartz and ${\alpha}$-Al2O3 were accelerated at 1300$^{\circ}C$. SiC was the main phase in the reaction product of acid-treated kaolin samples nitridated at 1300$^{\circ}C$ for 10 hours regardless of C/SiO2 ratio. But the XRD peak intensities of ${\beta}$-Si3N4, ${\beta}$-sialon and SiC did not show much difference when untreated raw kaolin was fired at the same condition. When the ratio of C/SiO2 was 3.5, ${\beta}$-sialon and ${\beta}$-Si3N4 existed in the reaction product of about 22% alumina containing kaolin sample fired at 1350$^{\circ}C$ for 7 hours. Only ${\beta}$-sialon existed in the same sample fired at 1400$^{\circ}C$ for 10 hours. ${\beta}$-sialon was obtained from all of the acid-treated kaolin samples fired at 1400$^{\circ}C$ for 40 hours, but AlN and SiC remained in the untreated kaolin sample. Z value of the ${\beta}$-sialon obtained from the 22% alumina containing kaolin sample fired at 1400$^{\circ}C$ for 40 hours was about 1.3(XRD) and 1.5(EDS). 2) Nitridation under 80N2+2OH2 mixed gas atmosphere with the C/SiO2 ratio of 1 Mullite was not found, but ${\alpha}$-Si3N4, and ${\beta}$-sialon were present in the reaction product of about 22% alumina containing kaolin sample fired at 1300$^{\circ}C$ for 10 hours. When untreated kaolin sample was nitridated at the same condition, mullite remained. AlN and SiC were not found in the reaction product of about 22% alumina containing kaolin sample fired at 1350$^{\circ}C$ for 5 hours. On the other hand, AlN and SiC remained in the product of untreated kaolin fired at the same condition.

• 한국재료학회지
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• 제2권6호
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• pp.408-416
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• 1992

Single-Si 기판과 poly-Si 기판에 각각 Ti을 sputter한 후 RTA 처리하여 안정한 TiS$i_2$를 형성하였다. 그 위에 Si이 1% 첨가된 Al-1% Si을 600nm sputter한 후 후속 열처리로서 400-60$0^{\circ}C$ 에서 30분간 $N_2$분위기로 furnace어닐링을 실시하였다. 이렇게 준비된 각 시편에 대하여 면저항 측정, Auger분석, SEM 사진으로 Al-1% Si/TiS$i_2$이중층 구조에서 Ti-silicide의 열적 안정성을 살펴 보았고, EDS 분석과 X-ray 회절 peak 분석을 통하여 Al-1% Si 층과 TiS$i_2$층의 반응으로 생긴 석출물의 성분과 상을 조사하였다. 이로 부터 다음과 같은 결과를 얻었다 Single-Si 기관에서 형성한 TiS$i_2$층은 Al-1% Si 층과 55$0^{\circ}C$에서 완전히 반응하여 석출물을 형성하였고, poly-Si 기판에서 형성한 TiS$i_2$층은 Al-1% Si 층과 50$0^{\circ}C$에서 완전히 반응하여 석출물을 형성하였는데 전반적으로 기판이 poly-Si인 경우가 반응이 더 잘 일어났고, 석출물의 크기도 비교적 컸다. 이는 poly-Si에 존재하는 grain boundary로 인해 poly-Si에서 형성된 Ti-silicide 층이single-Si 기관에서 형성된 Ti-silicide 층보다 불안정하기 때문으로 생각된다. EDS 분석에 의하여 석출물은 Ti, Al, 그리고 Si로 이루어진 3상 화합물이라고 추정되었고, X-ray회절 분석에 의해 석출물은 Ti, Al, 그리고 Si간의 3상 화합물인 T$i_7$A$l_5$S$i_12$로 확인되었다.