• Title/Summary/Keyword: crystal intensity

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Mineralogical Characterization of the Chuncheon Nephrite: Mineral Facies, Mineral Chemistry and Pyribole Structure (춘천 연옥 광물의 광물학적 특성 : 광물상, 광물 화학 및 혼성 격자 구조)

  • Noh, Jin Hwan;Cho, Hyen Goo
    • Journal of the Mineralogical Society of Korea
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    • v.6 no.2
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    • pp.57-79
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    • 1993
  • Chuncheon nephrite, which was formed by the polymetasomatic alteration of dolomitic marble, can be classified into pale green, green, dark green, and grey types on the basis of their occurrence, mineralogical and textural characteristics. The nephrites consist obiefly of fibrous or hairlike(length/width ratio>10) cryptocrystalline(crystal width < $2{\mu}m$) tremolite, and include less amounts of micro-crystalline diopside, calcite, clinochlore, and sphene as impurities. The oriented and rather curved crystal aggregate, of nephritic tremolite are densely interwoven, resulting in a massive-fibrous texture which may explain the characteristic toughness of nephritic jade. The characteristic greenish color of the nephrite may be preferably related to Fe rather than Cr and Ni. However, the variation of color and tint in the Chuncheon nephrite also depends on the mineralogical and textural differences such as crystallinity, texture, and impurities. The chemical composition of the nephritic tremolite is not stoichiometric and rather dispersed especially in the abundances of Al, Mg, and Ca. Al content and Mg/Ca ratio for the nephritic tremolite are slightly increased with deepening in greenish color of the nephrite. Fe content in the nephritic tremolite is generally very low, but comparatively richer in the dark green nephrite. In nephritic tremolite, wide-chain pyriboles are irregularly intervened between normal double chains, forming a chain-width disorder. Most nephritic tremolites in the Chuncheon nephrite show various type of chain-width defects such as triple chain(jimthompsonite), quintuple chain (chesterite), or sometimes quadruple chain in HRTEM observations. The degree of chain-width disorder in the nephritic tremolite tends to increase with deepening in greenish color. Triple chain is the most common type, and quadruple chain is rarely observed only in the grey nephrite. The presence of pyribole structure in the nephritic tremolite is closely related to the increase of Al content and Mg/Ca ratio, a rather dispersive chemical composition, a decrease of relative intensity in (001) XRD reflection, and an increase in b axis dimension of unit cell. In addition, the degree and variation of chain-width disorder with nephrite types may support that an increase of metastability was formed by a rapid diffusion of Mg-rich fluid during the nephrite formation.

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A Study of Coloration of Topaz(I): Mineralogical and Chemical Study on the Topaz Selected from Some Localities of the World (토파즈의 人工着色 處理를 위한 硏究(I) : 世界 主要 産地別 토파즈의 鑛物學的 및 化學的 特性)

  • Han, Yi-Kyeong;Park, Maeng-Eon;Jang, Yong-Nam
    • Journal of the Mineralogical Society of Korea
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    • v.5 no.2
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    • pp.109-121
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    • 1992
  • For the purpose of mineralogical and chemical study on the topazes from various localities of world(Brzail, China, India, Nigeria and Sri Lanka), electron microprobe analysis(EPMA), neutron activation analysis(NAA), X-ray diffractometry, Raman spectroscopy, etch test, scanning electron microscopy, refractive index, specific gravity, fluid inclusion were performed. The chemical composition in topaz was discussed along with its physical and structural properties. Variations in the unit-cell dimension and physical properties of topaz were found to have a close relations in the unit-cell dimension and physical properties of topaz were found to have a close relationship with extent of substitution of $OH^-\;for\;F^-$. According to neutron activation analyses, the trace elements had no effects on the physical properties of topaz. Raman spectra showed that the peaks of topaz were different in intensity from one locality to another. Etching defects in topaz includes negative crystal defect o point-bottom pit(India, Nigeria) and net work defect of curl-bottom pit(Brazil, China). Fluid inclusions in topaz may be classiffied into liquid $CO_2$-bearing inclusion, gaseous inclusion, halite, sylvite-bearing inclusion and liquid inclusion. The results of this study can be useful to devising artificial coloring methods for topaz with different mineralogical compositions.

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Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

The Crystal Structure of Cholesteryl Carbonates (콜레스테롤 카보네이트 결정구조에 관한 연구)

  • 박영자;신정미
    • Korean Journal of Crystallography
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    • v.7 no.1
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    • pp.8-19
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    • 1996
  • Cholestryl Methyl and Propyl Carbonate(CH3OCOOC27H45, C3H7OCOOC27H45) are monoclinic, space group P21, with a=17.014(1), b=7.682(1), c=10.612(1)Å, β=103.05(1)°, Z=2, V=1351.16Å3, Dc=1.09 g/cm3 for methyl carbonate, and with a=13.683(1), b=11.864(2), c=18.904(2)Å, β=106.30(1)°, Z=4, V=2945.4Å3, Dc=1.06 g/cm3, Dm=1.06 g/cm3 for propyl carbonate. The intensity data were collected on an Enraf-Nonius CAD-4 diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct methods and refined by full matrix least-squares methods. The final R factor was 0.051 for 2323 observed reflections for methyl carbonate and 0.074 for 3323 observed reflections for propyl carbonate. Compared with other cholesteryl derivatives, the cholesteryl ring and tail region of the molecules are normal. The molecules are stacked in clearly separated layers. At center of the layer, there are cholesteryl-C(17) side chain interactions. The interface region between layers is occupied by the loosely packed methyl carbonate chains. The structure of cholesteryl propyl carbonates have two propyl carbonates have two molecules(A, B) that are not related by crystal symmetry and have their tetracyclic system almost parallel to each other. Cholesteryl-cholesteryl interactions between symmetry related A-molecules, and cholesteryl-C(17) side chain interactions between symmetry related B-molecules occur at the center of the layers and these molecules stack along 2₁ screw axes. There are also C(17)chain-carbonate chain and C(17)chain-C(17)chain interactions in the interface region between layers. There is efficient packing between cholesteryl ring systems in propyl carbonates. Temperature ranges of cholesteric mesophases of cholesteryl alkyl cargonates are narrow for methyl, pentyl and hexyl carbonates, and rather broader for ethyl and propyl carbonates. Cholesteryl-isotropic transitions change very little with chain length.

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Treatment of N, P of Auto-Thermal Thermophilic Aerobic Digestion Filtrate with Struvite Crystallization (Struvite 결정화 반응을 이용한 고온 소화 여과액의 N, P 처리 특성)

  • Choo, Yeon-Duk;Kim, Keum-Yong;Ryu, Hong-Duck;Lee, Sang-Ill
    • Journal of Korean Society of Environmental Engineers
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    • v.33 no.11
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    • pp.783-789
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    • 2011
  • Recently, auto-thermal thermophilic aerobic digestion (ATAD) has a great attention for destruction of wasted sludge biomass in wastewater treatment plant. Reduction of sludge concentration has been successfully achieved with pilot scale ATAD and ceramic filtration process in field condition. However, high concentration of COD, total nitrogen (TN) and total phosphorus (TP) was observed in filtrate, which should be treated before recirculation of filtrate to biological wastewater treatment plant. This study was focused on removal of nitrogen and phosphorus contained in the filtrate of ATAD, using struvite crystallization method. The effect of operational and environmental parameters (such as, N, P and Mg ion concentration and molar ratio, pH, reaction time, agitation strength, seed dosage, and reaction temperature) on the treatment of TN and TP with struvite crystallization were evaluated. Magnesium (as $MgCl_26H_2O$) and phosphorus (as $K_2HPO_4$) ions were, if necessary, added to increase nitrogen removal efficiency by the crystal formation. Average concentration of $NH_4^+-N$ and $PO_4^{3-}-P$ of the filtrate were 1716.5 mg/L and 325.5 mg/L, respectively. Relationship between removal efficiencies of nitrogen and phosphorus and molar ratios of $Mg^{2+}$ and $PO_4^{3-}-P$ to $NH_4^+-N$ was examined. Crystal formation and nitrogen removal efficiencies were significantly increased as increasing molar ratios of magnesium and phosphorus to nitrogen. As molar ratio of $Mg^{2+}:PO_4^{3-}-P:NH_4^+-N$ were maintained to 2 : 1 : 1 and 2 : 2 : 1, removal efficiencies of nitrogen and phosphorus were 71.6% and 99.9%, and 93.8% and 98.6%, respectively. However, the effect of reaction time, mixing intensity, seed dose and temperature on the struvite crystallization reaction was not significant, comparing to those of molar ratios. Settled sludge volume after struvite crystallization was observed to be reduced with increase of seed dose and to be increased at high temperature.

Comparative Crystal Chemistry of Exchanged by Cs-, Cd-, Pb-, and Sr-synthetic Mordenite Using High Resolution X-ray Powder Diffraction (고분해능 X-선 분말 회절을 이용한 Cs-, Cd-, Pb-, Sr-으로 치환된 합성 모데나이트의 격자상수 비교 연구)

  • Lee, Soojin;Lee, Hyunseung;Seoung, Donghoon;Kim, Pyosang;Kim, Hyeonsu;Lee, Yongmoon
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.3
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    • pp.345-353
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    • 2022
  • This study aimed to fundamentally understand changes of cell parameters of cation-exchanged mordenites using high resolution X-ray powder diffraction for studies that immobilization of various heavy metal cation using synthesis mordenite (Na6.6Al6.6Si41.4O96·20.4H2O, Na-MOR). As a results of measurement by Thermogravimetric analysis (TGA), it was confirmed that 19.4, 20.4 water molecules per unit cell were present in monovalent-cation substituted MOR (Cs-MOR, Na-MOR), and 21, 23.1, 23.2 water molecules per unit cell were present in divalent-cation substituted MOR (Pb-MOR, Sr-MOR, Cd-MOR). The space group of all the samples were identified as Cmcm belonging to the orthorhombic crystal system. Compared to Na-MOR, starting material, relative peak intensity of (110) and (200) is significantly changed after cation substitution whereas peak position is almost similar. Also, (220) peak that was not found in Na-MOR was clearly observed in Pb-, Cd- and Sr-exchanged MOR. Thus, it was estimated that changes of atomic distribution usually occurred on ab-plane while changes of cell parameters were little. Detailed changes in the cell parameters of cation-exchanged mordenites were derived from whole profile fitting method using the GSAS suite program. Changes in the axial lengths and unit cell volume of cation substitution showed different relationship depending on ionic radius and charge number. In case of monovalent-cation substituted MOR, the length of a-axis increases whereas the length of b- and c-axis decrease by absorbed cation radius. In the case of divalent-cation exchanged MOR, the length of a-axis usually decreases while the length of b- and c-axis increases by cation radius. It was confirmed that unit cell volume of monovalent and divalent cation substituted MORs had an independent tendency by cation radius.

Luminescence Characterization of SrAl2O4:Ho3+ Green Phosphor Prepared by Spray Pyrolysis (분무열분해법으로 제조된 SrAl2O4:Ho3+ 녹색 형광체의 발광특성)

  • Jung, Kyeong Youl;Kim, Woo Hyun
    • Korean Chemical Engineering Research
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    • v.53 no.5
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    • pp.620-626
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    • 2015
  • $Ho^{3+}$ doped $SrAl_2O_4$ upconversion phosphor powders were synthesized by spray pyrolysis, and the crystallographic properties and luminescence characteristics were examined by varying activator concentrations and heattreatment temperatures. The effect of organic additives on the crystal structure and luminescent properties was also investigated. $SrAl_2O_4:Ho^{3+}$ powders showed intensive green emission due to the $^5F_4/^5S_2{\rightarrow}^5I_8$ transition of $Ho^{3+}$. The optimal $Ho^{3+}$ concentration in order to achieve the highest luminescence was 0.1%. Over this concentration, emission intensities were largely diminished via a concentration quenching due to dipole-dipole interaction between activator ions. According to the dependence of emission intensity on the pumping power of a laser diode, it was clear that the upconversion of $SrAl_2O_4:Ho^{3+}$ occurred via the ground state absorption-excited state absorption processes involving two near-IR photons. Synthesized powders were monoclinic as a major phase, having some hexagonal phase. The increase of heat-treatment temperatures from $1000^{\circ}C$ to $1350^{\circ}C$ led to crystallinity enhancement of monoclinic phase, reducing hexagonal phase. The hexagonal phase, however, did not disappear even at $1350^{\circ}C$. When both citric acid (CA) and ethylene glycol (EG) were added to the spray solution, the resulting powders had pure monoclinic phase without forming hexagonal phase, and led to largely enhancement of crystallinity. Also, N,N-Dimethylformamide (DMF) addition to the spray solution containing both CA and EG made it possible to effectively reduce the surface area of $SrAl_2O_4:Ho^{3+}$ powders. Consequently, the $SrAl_2O_4:Ho^{3+}$ powders prepared by using the spray solution containing CA/EG/DMF mixture as the organic additives showed about 168% improved luminescence compared to the phosphor prepared without organic additives. It was concluded that both the increased crystallinity of high-purity monoclinic phase and the decrease of surface area were attributed to the large enhancement of upconversion luminescence.

Chemical Age Dating of Zircon and Monazite by E1ectron Microprobe (전자현미분석기를 이용한 저어콘 및 모나자이트의 화학적 연대 측정법)

  • 이석훈
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.179-189
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    • 2001
  • The determination of trace concentration of U, Th and Pb was carried out for chemical dating of zircon and monazite by electron microprobe. Detection limit and error range should be considered to measure characteristic X-rays of M-line from those minerals, which are low in the ionization of atom and low peak intensity in the spectrum. The element of U, Th and Pb were simultaneously measured with 3 spectrometers equipped with PET crystal to reduce a total counting time and error due to drift of instrumental operating condition. Detection limit could be improved from increase of the peak/background ratio through adjusting pulse height analyzer about 1000 mv baseline. Under permissible maximum analytical conditions, theoretical detection limit of U, Th and Pb is down to 30 ppm (99% confidence level). The analytical result was maintained at a relative error $\pm$10% ($2{\sigma}$) in 800 ppm Pb, $\pm$5% ($2{\sigma}$) in 2330 ppm U and $\pm$10% ($2{\sigma}$) in dating from a single measurement of zircon at 15 keV and 100 nA. However, for the precise dating of zircon and monazite, if it is considered a 3 $\mu\textrm{m}$ spatial resolution, <100 ppm ($3{\sigma}$) detection limit and <$\pm$10% ($2{\sigma}$) relative error, optimum analytical conditions are given as 15~20 keV accelerating voltage, 100~200 nA beam current and 300~1200 sec total counting time. To reduce material damage by high current, there is need to be up to 3~5 $\mu\textrm{m}$ of electron beam diameter, or to use arithmetic average of multiple measuring at a shorter counting time. A younger or relatively low concentration rocks can be dated chemically by lower detection limit and improved precision resulted from increase of current and measuring time.

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Characterization of InAs Quantum Dots in InGaAsP Quantum Well Grown by MOCVD for 1.55 ${\mu}m$

  • Choe, Jang-Hui;Han, Won-Seok;Song, Jeong-Ho;Lee, Dong-Han
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.134-135
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    • 2011
  • 양자점은 전자와 양공을 3차원으로 속박 시키므로 기존의 bulk나 양자우물보다 양자점을 이용한 레이저 다이오드의 경우 낮은 문턱 전류, 높은 미분이득 및 온도 안전성의 장점이 있을 거라 기대되고 있다. 그러나, 양자점은 낮은 areal coverage 때문에 높은 속박효율을 얻지 못하고 있다. 이러한 양자점의 문제점을 해결하기 위해 양자점을 양자우물 안에 성장시켜 운반자들의 포획을 향상시키는 방법들이 연구되고 있다. 양자우물 안에 양자점을 넣으면 양자우물이 운반자들의 포획을 증가 시키고, 열적 방출도 억제하여 온도 안정성이 향상 되는 것으로 알려져 있다. 광통신 대역의 1.3 ${\mu}m$ 경우, GaAs계를 이용하여 InAs 양자점을 strained InGaAs 박막을 우물층으로 한 dot-in-a-well 구조의 연구는 몇몇 보고된 바 있다. 그러나 InP계를 사용하는 1.55 ${\mu}m$ 대역에서 dot-in-a-well구조의 연구는 아직 미미하다. 본 연구에서는 유기 금속 화학 증착법(metal organic chemical vapor deposition)을 이용하여 InP 기판 위에 InAs 양자점을 자발성장법으로 성장하였으며 dot-in-a-well 구조에서 우물층으로 1.35 ${\mu}m$ 파장의 $In_{0.69}Ga_{0.31}As_{0.67}P_{0.33}$ (1.35Q)를, 장벽층으로는 1.1 ${\mu}m$ 파장의 $In_{0.85}Ga_{0.15}As_{0.32}P_{0.68}$(1.1Q)를 사용하였다. 양자우물층과 장벽층은 모두 InP 기판과 격자가 일치하는 조건으로 성장하였다. III족 원료로는 trimethylindium (TMI)와 trimethylgalium (TMGa)을 사용하였으며 V족 원료 가스로는 $PH_3$ 100%, $AsH_3$ 100%를, carrier gas로는 $H_2$를 사용하였다. InP buffer층의 성장 온도는 640$^{\circ}C$이며 양자점 성장 온도는 520$^{\circ}C$이다. 양자점 형성은 원자력간 현미경(Atomic force microscopy)를 이용하여 확인하였으며, 박막의 결정성은 쌍결정 회절분석(Double crystal x-ray deffractometry)를 이용하여 확인하였다. 확인된 성장 조건을 이용하여 양자점 시료를 성장하였으며 광여기분광법(Photoluminescence)을 이용하여 광특성을 분석하였다. Fig. 1은 dot in a barrier 와 dot-in-a-well 시료의 성장구조이다. Fig. 1(a)는 일반적인 dot-in-a-barrier 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장한 후 양자점을 성장하였다. 그 후 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 1(b)는 dot-in-a-well 구조로 InP buffer층을 성장하고 1.1Q를 100 nm 성장 후 1.35Q 우물층을 4 nm 성장하였다. 그 위에 InAs 양자점을 성장하였다. 그 후에 1.35Q 우물층을 4 nm 성장하고 1.1Q 100 nm와 InP 100 nm로 capping하였다. Fig. 2는 dot-in-a-barrier 시료와 dot-in-a-well 시료의 상온 PL data이다. Dot-in-a-barrier 시료의 PL 파장은 1544 nm이며 반치폭은 79.70 meV이다. Dot-in-a-well 시료의 파장은 1546 nm이며 반치폭은 70.80 meV이다. 두 시료의 PL 파장 변화는 없으며, 반치폭은 dot-in-a-well 시료가 8.9 meV 감소하였다. Dot-in-a-well 시료의 PL peak 강도는 57% 증가하였으며 적분강도(integration intensity)는 45%가 증가하였다. PL 데이터에서 높은 에너지의 반치폭 변화는 없으며 낮은 에너지의 반치폭은 8 meV 감소하였다. 적분강도 증가에서 dot-in-a-well 구조가 dot-in-a-barrier 구조보다 전자-양공의 재결합이 증가한다는 것을 알 수 있으며, 반치폭 변화로부터 특히 높은 에너지를 갖는 작은 양자점에서의 재결합이 증가 된 것을 알 수 있다. 이는 양자우물이 장벽보다 전자-양공의 구속력을 증가시키기 때문에 양자점에 전자와 양공의 공급을 증가시키기 때문이다. 따라서 낮은 에너지를 가지는 양자점을 모두 채우고 높은 에너지를 가지는 양자점까지 채우게 되므로, 높은 에너지를 가지는 양자점에서의 전자-양공 재결합이 증가되었기 때문이다. 뿐만 아니라 파장 변화 없이 PL peak 강도와 적분강도가 증가하고 낮은 에너지 쪽의 반치폭이 감소한 것으로부터 에너지가 낮은 양자점보다는 에너지가 높은 양자점에서의 전자-양공 재결합율이 급증하였음을 알 수 있다. 우리는 이와 같은 연구에서 InP계를 이용해 1.55 ${\mu}m$에서도 dot in a well구조를 성장 하여 더 좋은 특성을 낼 수 있으며 앞으로 많은 연구가 필요할 것이라 생각한다.

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