• Bulletin of the Korean Chemical Society
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• v.33 no.4
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• pp.1141-1146
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• 2012

Ce-doped $Y_3Al_5O_{12}$ (YAG:Ce) phosphor powder was prepared using a ${NO_3}^-$-malonic acid-$NH_4NO_3-NH_3{\cdot}H_2O$ system. The YAG:Ce precursor was ignited at $240^{\circ}C$ and the resulting powder contained YAG:Ce crystallites (42%) - active in the visible region at 460 nm - amorphous particles (53%) - inactive at visible wavelengths - and less than 3% oxide (3%) crystallite impurities. The impurities transformed to acitive YAG:Ce crystallites at above $800^{\circ}C$. At above $1000^{\circ}C$, the amorphous phase became YAG phase and isolated $Ce_2O$ crystallites emerged. The powder particles comprised < $4{\mu}m$ secondary aggregates of 20 nm primary particles. The thermal dusting of the secondary particles coincided with the aggregation of the secondary particles at above $900^{\circ}C$.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.185-185
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• 2012

중공 발광 나노 물질은 특유의 구조적 특성(낮은 밀도, 높은 비표면적, 다공성 물질, 낮은 열팽창계수 등)과 광학적 성질을 이용하여 디스플레이 패널, 광결정, 약물전달체, 바이오 이미징 라벨 등의 다양한 적용이 가능하다. 이러한 적용에 있어 균일한 크기와 형태의 중공 입자는 필수 조건으로 여겨진다. 지금까지 합성된 중공 발광 입자에는 BaMgAl10O17 : Eu2+-Nd3+, Gd2O3 : Eu3+, $EuPO_4{\cdot}H_2O$과 같은 것들이 있으나 크기 조절이 어렵고, 그 균일성이 확보되지 못하였다. 균일한 크기의 중공 발광 입자를 만들기 위해 SiO2나 emulsion을 템플릿으로 이용하여 황화카드뮴, 카드뮴 셀레나이드 중공 입자를 합성한 예가 있으나, 양자점의 독성으로 인하여 바이오분야 응용에는 적합하지 않다. YAG는 모체로써 형광체에서 가장 많이 이용되는 물질로, 화학적 안정성과 낮은 독성, 높은 양자 효율 등 많은 장점을 갖고 있다. 특히 세륨이 도핑된 YAG형광체의 경우 WLED, 신틸레이터, 바이오산업에 적용이 가능하다. 그러나 지금까지 중공 YAG:Ce3+형광체를 합성한 예가 없었다. 본 연구에서는 단분산 수화 알루미늄 (Al(OH)3) 입자 위에 세륨이 도핑 된 이트륨 베이직 카보네이트 ($Y(OH)CO_3$)를 균일하게 코팅한 후 열처리를 하여 균일한 크기의 Y3Al5O12:Ce3+(YAG) 중공 입자를 합성하였다. 열처리 온도에 따른 고분해능 투과 전자 현미경(HRTEM), X-선 회절(XRD), 고분해능 에너지 분광법(HREDX) 분석결과, 중공 YAG: Ce3+입자는 Kirkendall 효과에 의해 형성됨을 확인하였다. 전계방사형 주사 전자 현미경(FE-SEM) 측정을 통해, 열처리 후에도 입자의 크기와 형태가 균일함을 확인하였으며, 공초점 현미경 관찰을 통해 중공 형태를 명확히 확인 할 수 있었다. Photoluminescence (PL) 분광법과 형광 수명 이미징 현미경(FLIM)을 이용한 광 특성 분석결과, 합성된 입자는 400-500 nm에서 흡수 파장 (456 nm에서 최대 강도)과 500-700 nm 범위의 발광 파장(544 nm에서 최대 강도)을 나타냈고, 상용 YAG: Ce3+(70 ns)에 준하는 74 ns의 잔광 시간(decay time)이 측정되었다. 단분산 수화 알루미늄 입자의 크기를 조절하여 최종 합성된 YAG: Ce3+의 크기를 조절할 수 있었다. 지름 약 600 nm의 Al(OH)3를 사용한 경우, $1,300^{\circ}C$에서 열처리를 한 후 평균 지름 590 nm의 중공입자를 합성하였고, 약 170 nm의 Al(OH)3를 이용하여, 더 낮은 온도인 $1,100^{\circ}C$에서의 열처리를 통해 평균지름 140 nm의 중공 YAG: Ce3+입자를 합성하였다. 본 연구를 통하여 합성된 균일한 크기의 YAG 중공입자는 LED와 같은 광전변환 소자 및 다기능성 바이오 이미징 등의 나노바이오 소자 분야에 활용될 수 있음이 기대된다.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.53 no.7
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• pp.352-357
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• 2004

The composites were fabricated, respectively, using 61vol.% SiC - 39vol.% TiB$_2$ and using 61vo1.% SiC - 39vo1.% WC powders with the liquid forming additives of 12wt% $Al_2$O$_3$＋Y$_2$O$_3$ by pressureless annealing at 180$0^{\circ}C$ for 4 hours. Reactions between SiC and transition metal TiB$_2$, WC were not observed in this microstructure. The result of phase analysis of composites by XRD revealed SiC(6H), TiB$_2$ and YAG(Al$_{5}$Y$_3$O$_{12}$) crystal phase on the SiC-TiB$_2$, and SiC(2H), WC and YAG(Al$_{5}$Y$_3$O$_{12}$) crystal phase on the SiC-WC composites. $\beta$\$\longrightarrow$$\alpha$-SiC phase transformation was ocurred on the SiC-TiB$_2$, but $\alpha$\$\longrightarrow$$\beta$-SiC reverse transformation was not occurred on the SiC-WC composites. The relative density, the vicker's hardness, the flexural strength and the fracture toughness showed respectively value of 96.2%, 13.34GPa, 310.19Mpa and 5.53Mpaㆍml/2 in SiC-WC composites. The electrical resistivity of the SiC-TiB$_2$ and the SiC-WC composites is all positive temperature coefficient resistance(PTCR) in the temperature ranges from $25^{\circ}C$ to 50$0^{\circ}C$. 2.64${\times}$10-2/$^{\circ}C$ of PTCR of SiC-WC was higher than 1.645${\times}$10-3/$^{\circ}C$ of SiC-TiB$_2$ composites.posites.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.49 no.9
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• pp.516-522
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• 2000

The mechanical and electrical properties of the hot-pressed and annealed $\beta-SiC-ZrB_2$ electroconductive ceramic composites were investigated as a function of the liquid forming additives of$Al_2O_3+Y_2O_3$ Phase analysis of composites by XRD revealed $\alpha-SiC(6H) ZrB_2\; and YAG(Al_5Y_3O_{12})$ The relative density of composites were increased with increased Al2O3+Y2O3 contents. The Flexural strength showed the highest value of 390.6MPa for composites added with 20wt% Al2O3+Y2O3 additives at room temperature. Owing to crack deflection crack bridging phase transition and YAG of fracture toughness mechanism the fracture toughness showed the highest value of 6.3MPa.m1/2 for composites added with 24wt% Al2O3+Y2O3 additives at room temperature. The resistance temperature coefficient showed the value of$ 2.46\times10^{-3}\;, 2.47\times10^{-3},\; 2.52\times10^{-3}/^{\circ}C$ for composite added with 16, 20, 24wt% Al2O3+Y2O3 additives respectively. The electrical resistivity of the composites was all positive temperature coefficient resistance(PTCR) in the temperature range of $256{\circ}C\; to\; 900^{\circ}C$.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.50 no.10
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• pp.500-503
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• 2001

The mechanical and electrical properties of the hot-pressed and pressureless annealed SiC+39vol.%$TiB_2$electroconductive ceramic composites were investigated as a function of the liquid additives of $Al_2O_3+Y_2O_3$. The result of phase analysis for the SiC+39vol.%$TiB_2$composites by XRD revealed $\alpha$-SiC(6H), $TiB_2$, and $YAG(Al_5Y_3O_{12})4 crystal phase. The relative density of SiC+39vol.%$TiB_2$ composites was increased with increased $Al_2O_3+Y_2O_3$. contents. The fracture toughness showed the highest value of $7.8 MPa.m^{1/2}$ for composites added with 12 wt % $Al_2O_3+Y_2O_3$. additives at room temperature. The electrical resistivity and the resistance temperature coefficient showed the lowest value of $7.3\times10_{-4}\Omega.cm\; and\; 3.8\times10_{-3}/^{\circ}C$ for composite added with 12 wt% $Al_2O_3+Y_2O_3$. additives at room temperature. The electrical resistivity of the SiC+39vol.%$TiB_2$composites was all positive temperature coefficient resistance(PTCR) in the temperature ranges from $25^{\circ}C\; to\; 700^{\circ}C$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.25 no.4
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• pp.166-171
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• 2015

In this study, using solid-state and flux, $Y_3Al_5O_{12}:Er^{3+}\;(YAG:Er^{3+})$ powders were successfully synthesized at low temperatures. To analyze the crystallinity of powders according to the synthesis or non-synthesis of powders and powder calcination temperatures, X-ray diffraction (XRD) was measured. In the case of pure YAG, when YAG was analyzed using the general solid-phase method, it was calcined for 12 hours at $1400^{\circ}C$ and pure YAG phase could be obtained. But when $BaF_2$ was added to YAG, YAG was synthesized at lower temperature (1000^{\circ}C$). It was thus found that the synthesis temperature could be lowered by about $400^{\circ}C$. Also, when BaF2 with an optimal concentration was added to $YAG:Er^{3+}$, the particle shape and size according to synthesis temperatures were surveyed, and corresponding luminous intensity was discussed.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.50 no.5
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• pp.221-225
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• 2001

The effect of $Al_2O_3+Y_2O_3$ additives on fracture toughness of ${\beta}-SiC-TiB_2$ composites by hot-pressed sintering was investigated. The ${\beta}-SiC-TiB_2$ ceramic composites were hot-press sintered and pressureless-annealed by adding 16, 20, 24 wt% ${\beta}-SiC-TiB_2$(6:4 wt%) powder as a liquid forming additives at low temperature(1800 $^{\circ}C$) for 4 h. Phase analysis of composites by XRD revealed mostly of ${\alpha}$-SiC(6H), $TiB_2$, and YAG($Al_5Y_3O_{12}$). The relative density was over 95-88 % of the theoretical density, and the porosity increased with increasing $Al_2O_3+Y_2O_3$ contents because of the increasing tendency of pore formation. The fracture toughness showed the highest value of 5.88 MPa${\cdot}m^{1/2}$ for composites added with 20 wt% $Al_2O_3+Y_2O_3$ additives at room temperature. The electrical resistivity showed the lowest value of $5.22{\times}10^{-4}\;{\Omega}\;{\cdot}\;cm$ for composite added with 20 wt% $Al_2O_3+Y_2O_3$ additives at room temperature, and was all positive temperature coefficeint resistance(PTCR) against temperature up to 900 $^{\circ}C$.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.53 no.5
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• pp.242-242
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• 2004

The composites were fabricated 61 vol.%α-α-SiC and 39vol.% WC powders with the liquid forming additives of 12wt% Al₂O₃＋Y₂O₃ by pressureless annealing at 1700, 1800, 1900℃ for 4 hours. The result of phase analysis of composites by XRD revealed α-SiC(2H), WC, and YAG($Al_5Y_3O_{12}$) crystal phase. The relative density, the flexural strength, fracture toughness and Young′s modulus showed respectively the highest value of 99.4%, 375.76㎫, 5.79㎫ㆍ$m^{\frac{1}{2}}$, and 106.43㎬ for composite by pressureless annealing temperature 1900℃ at room temperature. The electrical resistivity showed the lowest value of 1.47×$10^{-3}$/Ω·㎝ for composite by pressureless annealing temperature 1900℃ at 25℃. The electrical resistivity of the α-SiC-WC composites was all positive temperature cofficient resistance (PTCR) in the temperature ranges from 25℃ to 500℃.

• Korean Journal of Materials Research
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• v.30 no.11
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• pp.573-580
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• 2020

YAG (Yttrium Aluminum Garnet, Y₃Al₅O₁₂) has excellent plasma resistance and recently has been used as an alternative to Y₂O₃ as a chamber coating material in the semiconductor process. However, due to the presence of an impurity phase and difficulties in synthesis and densification, many studies on YAG are being conducted. In this study, YAG powder is synthesized by an organic-inorganic complex solution synthesis method using PVA polymer. The PVA solution is added to the sol in which the metal nitrate salts are dissolved, and the precursor is calcined into a porous and soft YAG powder. By controlling the molecular weight and the amount of PVA polymer, the effect on the particle size and particle shape of the synthesized YAG powder is evaluated. The sintering behavior of the YAG powder compact according to PVA type and grinding time is studied through an examination of its microstructure. Single phase YAG is synthesized at relatively low temperature of 1,000 ℃ and can be pulverized to sub-micron size by ball milling. In addition, sintered YAG with a relative density of about 98 % is obtained by sintering at 1,650 ℃.

• The Transactions of the Korean Institute of Electrical Engineers C
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• v.53 no.5
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• pp.241-247
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• 2004

The composites were fabricated 61 vol.%$\alpha$-$\alpha$-SiC and 39vol.% WC powders with the liquid forming additives of 12wt% $Al_2$O$_3$＋Y$_2$O$_3$ by pressureless annealing at 1700, 1800, 190$0^{\circ}C$ for 4 hours. The result of phase analysis of composites by XRD revealed $\alpha$-SiC(2H), WC, and YAG(Al$_{5}$ Y$_3$O$_{12}$ ) crystal phase. The relative density, the flexural strength, fracture toughness and Young's modulus showed respectively the highest value of 99.4%, 375.76㎫, 5.79㎫ㆍm$\frac{1}{2}$, and 106.43㎬ for composite by pressureless annealing temperature 190$0^{\circ}C$ at room temperature. The electrical resistivity showed the lowest value of 1.47${\times}$10$^{-3}$ $\Omega$$.$cm for composite by pressureless annealing temperature 190$0^{\circ}C$ at $25^{\circ}C$. The electrical resistivity of the $\alpha$-SiC-WC composites was all positive temperature cofficient resistance (PTCR) in the temperature ranges from $25^{\circ}C$ to 50$0^{\circ}C$.