Ba₂Mg(PO₄)₂:Eu 형광체의 합성과 자외선 여기하의 발광특성

태세원,정하균,최성호,허남회,Tae, Se-Won,Jung, Ha-Kyun,Choi, Sung-Ho,Hur, Nam-Hwi 한국재료학회 2008 한국재료학회지 Vol.18 No.11

For possible applications as luminescent materials for white-light emission using UV-LEDs, $Ba_2Mg(PO_4)_2:Eu^{2+}$ phosphors were prepared by a solid state reaction. The photoluminescence properties of the phosphor were investigated under ultraviolet ray (UV) excitation. The prepared phosphor powders were characterized to from a single phase of a monoclinic crystalline structure by a powder X-ray diffraction analysis. In the photoluminescence spectra, the $Ba_2Mg(PO_4)_2:Eu^{2+}$ phosphor showed an intense emission band centered at the 584 nm wavelength due to the f-d transition of the $Eu^{2+}$ activator. The optimum concentration of $Eu^{2+}$ activator in the $Ba_2Mg(PO_4)_2$ host, indicating the maximum emission intensity under the excitation of a 395 nm wavelength, was 5 at%. In addition, it was confirmed that the $Eu^{2+}$ ions are substituted at both $Ba^{2+}$ sites in the $Ba_2Mg(PO_4)_2$ crystal. On the other hand, the critical distance of energy transfer between $Eu^{2+}$ ions in the $Ba_2Mg(PO_4)_2$ host was evaluated to be approximately 19.3 A. With increasing temperature, the emission intensity of the $Ba_2Mg(PO_4)_2$:Eu phosphor was considerably decreased and the central wavelength of the emission peak was shifted toward a short wavelength.

PMMA 구를 주형으로 이용한 3DOM 전극 구조체의 제조

서경수,정하균,손용근,Seo Kyoung Soo,Jung Ha-Kyun,Son Yongkeun 한국재료학회 2004 한국재료학회지 Vol.14 No.8

Three-dimensionally ordered macroporous (3DOM) structures of the $LiCoO_2$ electrode materials for Li secondary batteries were fabricated by using the close-packed arrays of PMMA spheres served as templates. In order to successfully fabricate the cathode materials with highly ordered array form, the metal citrates were applied to new precursors. The precursor/template composites were prepared by the infiltration with metal citrate precursors into the voids of template. By removing the PMMA templates, then, the inverse opal structures with the uniform pores of narrow size distribution were resulted. It was confirmed that the 3DOM $LiCoO_2$ material is to take a single phase of rocksalt (R3m) structure. In addition, 3DOM $LiNiO_2$ and $LiMn_{2}O_4$ cathode materials were fabricated using an identical preparation procedure. Also, the morphology of the 3DOM cathode materials calcined at $500^{\circ}C\;to\;700^{\circ}C$ was observed by scanning electron microscope.

다단 침전법에 의한 구형 BaMgAl₁₀O₁₇:Eu 형광체의 제조 및 특성

박정민,정하균,박희동,박윤창,Park, Jumg-Min,Jung, Ha-Kyun,Park, Hee-Dong,Park, Yoon-Chang 한국재료학회 2002 한국재료학회지 Vol.12 No.11

A spherical $BaMgAl_{10}$ $O_{17}$ :Eu phosphor has been synthesized by a multi-step precipitation route. In order to successfully synthesize the phosphor with spherical shape, the hydrated-alumina particles should be controlled for spherical shape. In this process, the hydroxypropyl cellulose (HPC) was used as a dispersing reagent. This reagent plays an important role in that the particles were controlled to have the uniform size of sub-micron. The final product prepared by the multi-step precipitation method maintained spherical shape with uniform size of 0.4$\mu\textrm{m}$. It can be seen in X-ray diffraction patterns, formation of the single phase of $BaMgAl_{10}$ $O_{17}$ :Eu phosphor prepared by the multi-step precipitation method at $1350^{\circ}C$. Also, the emission spectra of spherical $BaMgAl_{O}$ $10_{17}$ :Eu phosphor in the present case was compared with those of commercially-available blue phosphor under VUV (Vacuum Ultra Violet) excitation. The luminescence process of the $BaMgAl_{10}$ $O_{17}$ :Eu phosphor is characterized by the $4f^{6}$$5d^1$longrightarrow4f$^{7}$ transition (blue) of the $Eu^{2+}$ ion acting as an activating center and the maximum luminescence intensity was obtained by reduction treatment at 145$0^{\circ}C$.

새로운 $Mg_{2}SnO_{4}:Mn$ 형광체의 광 발광 특성

김경남,정하균,박희동,김도진,Kim, Kyung-Nam,Jung, Ha-Kyun,Park, Hee-Dong,Kim, Do-Jin 한국세라믹학회 2001 한국세라믹학회지 Vol.38 No.9

A new $Mg_{2-x}MN_xSnO_4$ phosphor with an inverse spinel structure was synthesized by the solid-state reaction technique. The photoluminescence properties of the $Mg_2SnO_4$:Mn phosphors were investigated under 147nm -vacuum ultraviolet ray excitation. The Mn-doped $Mg_2SnO_4$ phosphor exhibited high emission intensity with the spectrum centered at 500nm wavelength. It was explained that the green emission in $Mg_2SnO_4$:Mn phosphor has originated from energy transfer from $^4T_1$ to $^6A_1$ of $Mn^{2+}$ ion at tetrahedral site of the spinel structure. The $Mn^{2+}$ ion concentration exhibiting the maximum emission intensity under the excitation of 147nm-vacuum ultraviolet ray was 0.25mol%. And the decay time of the phosphor was shorter than 10ms. 새로운 형광체로 역스피넬 구조를 갖는 $Mg_{2-x}MN_xSnO_4$ 조성을 선정하여 고상반응에 의하여 제조하였다. $Mg_2SnO_4:Mn$의 광발광 특성이 147nm 파장의 진공 자외선 여기하에 측정되었다. Mn의 첨가에 의하여 $Mg_2SnO_4$ 형광체는 500nm 파장에 발광 중심을 가지며 매우 높은 발광강도를 나타내었다. 이것은 스피넬 구조의 산소 사면체 배위에 위치하는 Mg 자리를 치환하여 들어가는 $Mn^{2+}$ 이온의 $^4T_1$ 상태로부터 $^6A_1$ 상태로의 에너지 전이에 의한 발광으로 해석되었다. 진공 자외선 여기하에 최대의 발광강도를 나타내는 Mn 활성제의 농도는 0.25mol%이었고, 잔광시간은 10ms 이하인 것으로 조사되었다.

수열합성에 의해 제조된 YVO₄:Eu³⁺ 형광체의 발광특성

문영민,최성호,정하균,임상호,Moon, Yong-Min,Choi, Sung-Ho,Jung, Ha-Kyun,Lim, Sang-Ho 한국재료학회 2008 한국재료학회지 Vol.18 No.10

We have synthesized $Eu^{3+}$-doped $YVO_4$ phosphors by using a hydrothermal method and investigated their luminescent properties. Aqueous solutions of $Y_2O_3,\;V_2O_5,\;Eu_2O_3$, and nitric acid with various pH values were used as the precursors. The crystallinity, surface condition, and emission characteristics were examined using XRD, FT-IR, and photo-excited spectrometer. $Eu^{3+}$ incorporation followed by the efficient red emission strongly depends on the acidity of solution media. The emission intensity becomes stronger as the pH values increase to 7 and then gradually decreases. This phenomenon might be related to the hydroxyl quenching effect, which is induced by surface bound OH-groups.

진공자외선 여기에 의한 YAGG:Ce³⁺ 형광체의 광발광 특성에 미치는 Al₂O₃ 나노입자 원료의 결정상의 영향

우미혜,최성호,정하균,Wu, Mi-Hye,Choi, Sung-Ho,Jung, Ha-Kyun 한국재료학회 2012 한국재료학회지 Vol.22 No.4

$Ce^{3+}$-doped yttrium aluminum gallium garnet (YAGG:$Ce^{3+}$), which is a green-emitting phosphor, was synthesized by solid state reaction using ${\alpha}$-phase or ${\gamma}$-phase of nano-sized $Al_2O_3$ as the Al source. The processing conditions and the chemical composition of phosphor for the maximum emission intensity were optimized on the basis of emission intensity under vacuum UV excitation. The optimum heating temperature for phosphor preparation was $1550^{\circ}C$. Photoluminescence properties of the synthesized phosphor were investigated in detail. From the excitation and emission spectra, it was confirmed that the YAGG:$Ce^{3+}$ phosphors effectively absorb the vacuum UV of 120-200 nm and emit green light positioned around 530 nm. The crystalline phase of the alumina nanoparticles affected the particle size and the luminescence property of the synthesized phosphors. Nano-sized ${\gamma}-Al_2O_3$ was more effective for the achievement of higher emission intensity than was nano-sized ${\alpha}-Al_2O_3$. This discrepancy is considered to be because the diffusion of $Al^{3+}$ into $Y_2O_3$ lattice is dependent on the crystalline phase of $Al_2O_3$, which affects the phase transformation of YAGG:$Ce^{3+}$ phosphors. The optimum chemical composition, having the maximum emission intensity, was $(Y_{2.98}Ce_{0.02})(Al_{2.8}Ga_{1.8})O_{11.4}$ prepared with ${\gamma}-Al_2O_3$. On the other hand, the decay time of the YAGG:$Ce^{3+}$ phosphors, irrespective of the crystalline phase of the nano-sized alumina source, was below 1 ms due to the allowed $5d{\rightarrow}4f$ transition of the $Ce^{3+}$ activator.

색순도가 우수한 갈륨 산화물계 적색 형광체의 광발광 특성

김경운,최성호,정하균,남산,Kim, Kyoung-Un,Choi, Sung-Ho,Jung, Ha-Kyun,Nahm, Sahn 한국재료학회 2008 한국재료학회지 Vol.18 No.3

$Eu^{3+}$-activated $R_3GaO_6$ (R = Y, Gd) phosphors were prepared in a conventional solid-state reaction and their optical properties were investigated. These compounds exhibit strong red emission under light excitation at 254 nm. The emission spectra are dominated by peaks appearing around 610-630 nm that are induced by the electric dipole transition of $^5D_0\;{\rightarrow}\;^7F_2$ of $Eu^{3+}$. In addition, the appropriate CIE (Commission Internationale de l'clairage) chromaticity coordinates, (x = 0.656, y = 0.336) for $Y_3GaO_6$ and (x = 0.655, y = 0.334) for $Gd_3GaO_6$, become closer to the NTSC (National Television System Committee) standard values. With the optimized activator concentrations, the maximum emission brightness is approximately 80% of $Y_2O_3$:$Eu^{3+}$ typical red-emitting phosphor with improved color purity under an excitation condition of 254 nm.

분무열분해법에 의해 제조된(Ca, Sr)₂MgSi₂O₇:Eu²⁺ 형광체의 발광 특성

이호민,정경열,정하균,이종흔,Lee, Ho Min,Jung, Kyeong Youl,Jung, Ha-Kyun,Lee, Jong Heun 한국화학공학회 2006 Korean Chemical Engineering Research(HWAHAK KONGHA Vol. No.

분무열분해법을 이용하여$(Ca,Sr)_{2-y}MgSi_2O_7:Eu^{2+}{_y}$ 형광체 분말을 제조하고 $Eu^{2+}$의 농도, 후열처리온도 변화 및 Ca/Sr 비에 따른 발광특성을 조사하였다. 또한, Ca/Sr의 비를 변화시켜 발광특성의 변화를 관찰하였다. $Ca_2MgSi_2O_7$나 $Sr_2MgSi_2O_7$ 분말 모두 $1,000^{\circ}C$ 이상의 온도에서 열처리를 했을 때 순수한 정방정계 상이 제조되었다. $Ca_2MgSi_2O_7:Eu^{2+}{_y}$ 녹색 형광체는 $Eu^{2+}(y)$의 농도가 5 mol%, 후열처리 온도가 $1,250^{\circ}C$ 일 때 가장 높은 발광 강도는 보였다. ${(Ca_{1-x},Sr_x)}_{1.95}MgSi_2O_7:{Eu^{2+}}_{0.05}$의 발광 파장은 Sr의 농도가 증가함에 따른 결정장 감소로 인해 524nm에서 456nm로 점진적으로 blue shift 되었다. $Sr_2MgSi_2O_7:Eu^{2+}$는 Sr 자리에 약 10 mol% Ca를 치환시킴으로써 청색 형광체의 발광 강도는 크게 향상되었다. 제조된 분말들은 치밀하지 못하고 다공성 구조를 가져 후열처리 전에는 구형을 유지하였으나 열처리($900{\sim}1,300^{\circ}C$) 후에는 구형의 형상을 잃고 입자들 간의 응집이 발생하였다. $(Ca,Sr)_{2-y}MgSi_2O_7:Eu^{2+}{_y}$ (CMS) phosphor particles were prepared by using a spray pyrolysis process. The luminescent property was optimized by changing the content of Eu and the post-treatment temperature. The luminescence characteristics were also monitored with changing the ratio of Ca to Sr. The pure tetragonal $Ca_2MgSi_2O_7$ or $Sr_2MgSi_2O_7$ particles were obtained when the post-treatment temperature was over $1,000^{\circ}C$. The highest emission intensity of CMS particles were achieved when the concentration (y) of Eu and the treatment temperature were 0.05 and $1,250^{\circ}C$,respectively. The emission wavelength $({\lambda}_{max})$ of ${(Ca_{1-x},Sr_x)}_{1.95}MgSi_2O_7:{Eu^{2+}}_{0.05}$ was gradually shifted from 524 nm to 456 nm with increasing the content of Sr due to the reduction of crystal field strength. The emission intensity and its width of $Sr_2MgSi_2O_7:Eu$ was greatly enhanced by substituting Ca of less than 10 mol% for Sr without any significant peak shift. The morphology of as-prepared particles was spherical, but changed to irregular-shaped one after the post treatment at the temperature range from 900 at $1,300^{\circ}C$.

적색 발광 (Y,Al)VO₄:Eu³⁺ 형광체 나노입자의 합성과 발광 특성

서정현,최성호,남산,정하균,Seo, Jung-Hyun,Choi, Sung-Ho,Nahm, Sahn,Jung, Ha-Kyun 한국재료학회 2012 한국재료학회지 Vol.22 No.2

Red-emitting $Eu^{3+}$-activated $(Y_{0.95-x}Al_x)VO_4$ (0 < x $\leq$ 0.12) nanophosphors with the particle size of ~30 nm and the high crystallinity have been successfully synthesized by a hydrothermal reaction. In the synthetic process, deionized water as a solvent and ethylene glycol as a capping agent were used. The crystalline phase, particle morphology, and the photoluminescence properties of the excitation spectrum, emission intensity, color coordinates and decay time, of the prepared $(Y_{0.95-x}Al_x)VO_4:Eu^{3+}$ nanophosphors were compared with those of the $YVO_4:Eu^{3+}$. Under 147 nm excitation, $(Y_{0.95-x}Al_x)VO_4$ nanophosphors showed strong red luminescence due to the $^5D_0-^7F_2$ transition of $Eu^{3+}$ at 619 nm. The luminescence intensity of $YVO_4:Eu^{3+}$ enhanced with partial substitution of $Al^{3+}$ for $Y^{3+}$ and the maximum emission intensity was accomplished at the $Al^{3+}$ content of 10 mol%. By the addition of $Al^{3+}$, decay time of the $(Y,Al)VO_4:Eu^{3+}$ nanophosphor was decreased in comparison with that of the $YVO_4:Eu^{3+}$ nanophosphor. Also, the substitution of $Al^{3+}$ for $Y^{3+}$ invited the improvement of color coordinates due to the increase of R/O ratio in emission intensity. For the formation of transparent layer, the red nanophosphors were fabricated to the paste with ethyl celluloses, anhydrous terpineol, ethanol and deionized water. By screen printing method, a transparent red phosphor layer was formed onto a glass substrate from the paste. The transparent red phosphor layer exhibited the red emission at 619 nm under 147 nm excitation and the transmittance of ~80% at 600 nm.

희토류 이온(Er/Yb)이 도핑된 LaPO₄ 나노입자의 합성과 발광특성

오재석,이택혁,석상일,정하균,Oh Jae-Suk,Lee Tack-Hyuck,Seok Sang-Il,Jung Ha-Kyun 한국재료학회 2004 한국재료학회지 Vol.14 No.4

Due to the luminescence by$ Er ^{ 3+}$ activator, Er-doped $LaPO_4$ powders can be applied for optical amplification materials. In this study, $LaPO_4$:Er nanoparticles were synthesized in solution system using a high-boiling coordinating solvent and their properties were investigated through various spectroscopic techniques. The nanoparticles were to take a single phase of monazite structure by a X-ray diffraction analysis and to have the 5-6 nm of particles size with narrow size distribution by a TEM. And it was confirmed by the EA and FT-IR analyses that the surfaces of nanoparticles are coordinated with the solvent molecules, which will possibly keep from agglomerating between LaPO$_4$:Er nanoparticles. In the emission spectrum of $LaPO_4$:Er nanoparticle at NIR region, on the other hand, it was measured that the emission intensity is very weak, which is due to the transition from $^4$$I_{(13/2)}$ to $^4$$I_{(15/2)}$ of $Er^{3+ }$ion. It was interpreted that the weak luminescence of $LaPO_4$:Er is originated from the hydroxyl groups adsorbed on the surfaces of the nanoparticles, because OH group acts as an efficient quencher for the $^4$$I_{(13/2)}$ \longrightarrow $^4$$I_{(15/2)}$ emission of $Er^{3+}$ activator. But the co-doping of Yb$^{3+}$ as a sensitizer in this nanoparticle results in the increase of the emission intensity at 1539 nm due to the effective energy transfer from $Yb^{3+}$ to $Er^{3+}$ . In addition, the synthesized nanoparticles exhibited good dispersibility with some polymers and effective luminescence at NIR region.n.