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All-In-One Light-Tunable Borated Phosphors with Chemical And Research Article www.acsami.org All-In-One Light-Tunable Borated Phosphors with Chemical and Luminescence Dynamical Control Resolution † ‡ § ‡ ∥ ⊥ Chun Che Lin, Yun-Ping Liu, Zhi Ren Xiao, Yin-Kuo Wang, , Bing-Ming Cheng, † # ○ and Ru-Shi Liu*, , , † Department of Chemistry, National Taiwan University, Taipei 106, Taiwan ‡ Department of Physics, National Taiwan Normal University, Taipei 106, Taiwan § Graduate Institute of Applied Physics, National Chengchi University, Taipei 116, Taiwan ∥ Center for General Education and Department of Physics, National Taiwan Normal University, Taipei 106, Taiwan ⊥ National Synchrotron Radiation Research Center, Hsinchu 300, Taiwan # Department of Mechanical Engineering, National Taipei University of Technology, Taipei 10608, Taiwan ○ Graduate Institute of Manufacturing Technology, National Taipei University of Technology, Taipei 10608, Taiwan *S Supporting Information ABSTRACT: Single-composition white-emitting phosphors with supe- rior intrinsic properties upon excitation by ultraviolet light-emitting diodes are important constituents of next-generation light sources. 3+ 3+ Borate-based phosphors, such as NaSrBO3:Ce and NaCaBO3:Ce , have stronger absorptions in the near-ultraviolet region as well as better chemical/physical stability than oxides. Energy transfer effects from sensitizer to activator caused by rare-earth ions are mainly found in the obtained photoluminescence spectra and lifetime. The interactive mechanisms of multiple dopants are ambiguous in most cases. We 3+ 3+ adjust the doping concentration in NaSrBO3:RE (RE = Ce ,Tb , Mn2+) to study the energy transfer effects of Ce3+ to Tb3+ and Mn2+ by comparing the experimental data and theoretical calculation. The vacuum-ultraviolet experimental determination of the electronic energy levels for Ce3+ and Tb3+ in the borate host regarding the 4f−5d and 4f− 4f configurations are described. Evaluation of the Ce3+/Mn2+ intensity ratios as a function of Mn2+ concentration is based on the analysis of the luminescence dynamical process and fluorescence lifetime measurements. The results closely agree with those directly obtained from the emission spectra. Density functional calculations are performed using the generalized gradient approximation plus an on-site Coulombic interaction correction scheme to investigate the forbidden mechanism of interatomic 3+ 2+ 3+ 3+ 2+ energy transfer between the NaSrBO3:Ce and NaSrBO3:Eu systems. Results indicate that the NaSrBO3:Ce ,Tb , and Mn phosphors can be used as a novel white-emitting component of UV radiation-excited devices. KEYWORDS: white-emitting phosphors, energy transfer effects, DFT investigations, devices 1. INTRODUCTION 410 nm) with blue/green/red tricolor phosphors because these Since the incorporation of Ce-doped yttrium aluminum garnet provide high color rendering indexes and excellent light output (Y Al O :Ce3+; abbreviated as YAG:Ce3+) as a vivacious performances. However, the considerable reabsorption causes 3 5 12 low luminescent efficiency, and the complicated design of emission layer for the fabrication of white light-emitting diodes 9,10 (w-LEDs) by the Nichia Corporation, the performance of multiple emitting components are rugged in this system. In phosphor-converted LED (pc-LED) has been improved mainly recent years, researchers have been developing single- by diversifying the components and encapsulation of the device composition white-emitting phosphors, which are excited by − as well as phosphor synthesis and architecture refinement.1 3 UV-LED to prevent the cross-color, instability of color Diverse approaches have been explored to enhance w-LED temperature, and expensive cost problems. Even though the efficiency, such as by improving the chips, electric circuits, phosphor is an important component of the LED device, phosphors, and encapsulants.4,5 Moreover, chromatic aberra- relatively scant studies have been conducted on the interactive tion and thermal quenching prevent the expansion of the most common w-LED composed of an InGaN-based blue diode and Received: March 3, 2014 − yellow YAG:Ce3+ phosphor.6 8 An alternative way to overcome Accepted: May 20, 2014 these difficulties is to combine ultraviolet (UV) LEDs (300 to Published: May 20, 2014 © 2014 American Chemical Society 9160 dx.doi.org/10.1021/am501232y | ACS Appl. Mater. Interfaces 2014, 6, 9160−9172 ACS Applied Materials & Interfaces Research Article mechanism of the activators. Therefore, determination of the Particularly, the energy transfer of Ce3+ → Eu2+ is absent in the ff importance of the energy transfer e ects in luminescent NaSrBO3 system based on the theoretical calculation experi- 3+ 3+ 2+ materials depends on experimental results and also theoretical ment. The as-prepared NaSrBO3:RE (RE = Ce ,Tb ,Mn ) calculations.11 First, energy transfer from vicinal sensitizers has phosphors can generate white light for practical UV-LED been considered to enhance or quench the improvement of the devices. We have also constructed a significant model to explain emission intensity in various activators. For instance, the broad a possible mechanism of interatomic energy transfer between emission band in the visible range of the transition metal Mn2+ rare-earth ions. From our study, it is clearly found that the − 3+ 3+ 2+ originates from the d d transition consisting of a forbidden NaSrBO3:RE (RE = Ce ,Tb ,Mn ) phosphors have high transition and difficult excitation. For this reason, the distinct emission intensity and better thermal stability as compared with 2+ 3+ 3+ 2+ emission of Mn ions is usually excited through energy transfer the NaCaBO3: RE (RE = Ce ,Tb ,Mn ) demonstrated by from the spectral overlap between the absorption band of Mn2+ Zhang et al.35 ions and the emission band of promising sensitizer Eu2+ or Ce3+ 12−19 ions in many hosts. Second, considering the practical 2. EXPERIMENTAL SECTION applications of LED devices, the excitation wavelength of the 2.1. Materials and Synthesis. activators cannot match the requirements of the available chips. A series of borate-based NaSr − − − BO :Ce ,Tb,Mn compounds with versatile dopants For example, the rigorously forbidden 4f−4f transitions of the 1 x y z 3 x y z 3+ were synthesized in one step by the solid-state reaction. The high- Tb absorption peaks in the near UV region are very weak. purity Na CO (Crown Guaranteed Reagents, 99.7%), SrCO 2+ 3+ 2 3 3 Some favorable ions such as Eu and Ce , whose electric (Aldrich, 99.99%), H BO (Riedel-de Haen,̋ 99.8%), CeO (Aldrich, fi 3 3 2 dipole-allowed transition commonly engages bene cially in the 99.995%), Tb4O7 (Aldrich, 99.99%), and Mn2O3 (Aldrich, 99%) were UV- or blue-chip, can work as a helpful energy donor (D) in used as precursors in stoichiometric mixtures. Precise amounts of the which the efficient energy transfer occurs between D and the starting materials were weighed out and ground in an agate mortar for − energy acceptor (A).20 27 According to Dexter’senergy- 30 min to obtain homogeneous mixtures. The mixtures were placed in ffi alumina crucibles and were then sintered at 850 °C for 8 h at a heating transfer theory, the determination of e ciency principally ° rate of 5 C/min under a reducing atmosphere (N2/H2 = 95:5) in an depends on the spectral overlap between the emission spectra fi 28 electric tube furnace. After ring, the samples were gradually cooled to of the sensitizers and the absorption spectra of the activators. room temperature in the furnace. The products were crushed and Co-doped phosphor accompanied two kinds of transfer prepared for measurements. pathways: nonradiative and radiative. The nonradiative transfer 2.2. Characterization. The composition and phase purity of the mechanism is confusing because of the unknown multipolar products were identified using synchrotron X-ray diffraction (SXRD) interaction and exchange interaction.11 Furthermore, the broad patterns. A wavelength of λ = 0.774907 Å was recorded using a emission energy transition (5d → 4f) of the sensitizers, which is Debye−Scherrer camera installed at the BL01C2 beamline of the ff National Synchrotron Radiation Research Center (NSRRC) in allowed by the Laporte parity selection rules, is deeply a ected fi by the crystal field and the covalency of many inorganic hosts.29 Hsinchu, Taiwan. X-ray Rietveld re nement of the structural models 30 and texture analysis were performed using the General Structure Wu et al. successfully synthesized a novel orthoborate Analysis System (GSAS)37 software. Photoluminescence excitation (NaSrBO3) that was crystallized in the monoclinic space group (PLE) and emission (PL) spectra were measured using the P21/c consisting of the anisotropic polarizations of planar BO3 FluoroMax-3 and FluoroMax-P spectrophotometers equipped with a groups, according to the powder X-ray diffraction data. This 150 W Xe lamp and a Hamamatsu R928 photomultiplier tube. The chemical composition has good quantum efficiency (QE), high quantum efficiency (QE) was measured by the absolute method in color purity, low reaction temperature, and good stability when HORIBA Jobin-Yvon spectrofluorimeters. An optical integrating − doped with rare-earth activators.31 34 After our previous sphere (diameter of 100 mm) showed a reflectance >99% over − − submission, Zhang et al.35,36 reported the luminescence of 400 1500 nm range (>95% within 250 2500 nm) in the device. The 3+ accessories were made from Teflon (rod and sample holders) or single-doped phosphor NaCaBO3:Ce and the color/chroma- ffl 3+ 3+ Spectralon (ba e). VUV PLE and PL spectra were obtained using a ticity tenability of multidoped phosphor NaCaBO3:Ce ,Tb , 2+ 3+ 3+ beamline BL03A at NSRRC. The PLE spectra were obtained by and Mn with the energy transfer processes of Ce to Tb scanning a 6 m cylindrical grating (450 grooves/mm) monochroma- 2+ and Mn . Here, we demonstrate the parameters of borate tor, which has a spanning wavelength range of 85 to 350 nm. A CaF ’ 2 crystallography (NaSrBO3) in detail where Sr s are replaced by plate with a cutoff wavelength at approximately 123 nm was used as a dopants. Moreover, we report the luminescent and energy filter to remove the high-order light from the synchrotron.
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