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Preparation method of blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder

A nano-fluorescent powder and near-ultraviolet technology, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of poor doping uniformity and particle size uniformity, difficult control of surface defects, and poor safety performance. Good stability, high uniformity of phase, and the effect of ensuring safe production

Active Publication Date: 2013-04-24
CENT SOUTH UNIV
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Problems solved by technology

[0003] Aiming at the general problems existing in the commercialized three-primary-color phosphors, people have developed a single-matrix panchromatic phosphor, but with the deepening of research and wide application, it has been found that the single-matrix panchromatic phosphor has the following problems: (1 ). Panchromatic phosphors are mainly concentrated in ultraviolet or near-ultraviolet LED excitation types, while blue LED excitation types are relatively scarce, which is inconsistent with the current mainstream trend of blue LED chips; (2). Phosphor powder excitation spectrum and LED emission spectrum cannot Very good matching, resulting in low light conversion efficiency, large light loss, and directly affect the light intensity of white LEDs; (3). The peak intensity ratio of the three primary colors is not suitable, and there are phenomena such as lack or shortage of red components, which affect the white LED. The color rendering index cannot meet the lighting requirements; (4). The room for improving the quantum efficiency and luminous intensity is low. In order to make up for these shortcomings, the following three methods are adopted at home and abroad:
[0008] Traditional full-color phosphors generally use high-temperature solid-phase method, which has defects such as low doping concentration, poor doping uniformity and particle size uniformity, high sintering temperature, high energy consumption, high cost, and difficulty in forming nanoscale matrix.
The preparation of micro / nano-particle three-color phosphors generally adopts the sol-gel method, although the sol-gel method has: (a) low operating temperature; (b) easy to accurately control the doping amount; (c) can avoid the experimental The introduction of impurities maintains the purity of the sample; (d) the precursor solution is mixed at low temperature and can achieve a high degree of uniformity at the molecular level, but there are also the following disadvantages: (a) the entire sol-gel process requires It takes a long time and often takes several days or weeks; (b) the final product still needs a calcination process to obtain, which increases the production cycle and cost; (c) there are a large number of micropores in the gel, and the calcined Many gases and harmful gases such as organic matter will escape, and shrinkage and agglomeration will occur. After calcination, the particles will grow up and the sintering performance will be poor.
(d) The prepared phosphor is granular, and the surface defects are difficult to control
The hydrothermal method is a new method developed in recent years for the preparation of one-dimensional nanomaterials. It has: (a) easy operation; (b) sufficient conversion of raw materials; (c) can form a special high temperature and high pressure environment, making it difficult to The characteristics of soluble or insoluble substances are dissolved and recrystallized. By controlling the molar ratio of raw materials, reaction temperature, reaction time and filling degree, it is very convenient to synthesize large-scale one-dimensional nanomaterials with uniform diameter distribution. However, hydrothermal There are relatively few studies on the preparation of phosphors by the hydrothermal method, mainly because the hydrothermal method is generally carried out under high temperature and high pressure, and the requirements for equipment are relatively high, the technology is difficult, and the safety performance is poor.
[0009] At present, there is no report on the preparation of one-dimensional nano-phosphor powder by sol-hydrothermal method

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  • Preparation method of blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder
  • Preparation method of blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder
  • Preparation method of blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder

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Effect test

Embodiment 1

[0050] Embodiment 1. 1.046g GeO 2 , 0.3976g CaO, 0.8018g europium acetate tetrahydrate, 0.453g terbium nitrate hexahydrate mixed with 120ml deionized water, after ultrasonic treatment for 60min, moved into a 200ml polytetrafluoroethylene reactor, placed in a heating furnace, at 200 ℃ temperature conditions for 24 hours. After the reaction was completed, it was naturally cooled to room temperature. Take it out and dry it in a drying oven at 90°C to obtain a one-dimensional linear full-color nano-fluorescent powder with a diameter of about 10-80 nm and a length of 30-1000 microns.

Embodiment 2

[0051] Embodiment 2. 1.046g GeO 2 , 0.3976g CaO, 0.8018g europium acetate tetrahydrate, 0.453g terbium nitrate hexahydrate mixed with 120ml deionized water, after ultrasonic treatment for 45min, moved into a 200ml polytetrafluoroethylene reactor, placed in a heating furnace, at 100 ℃ temperature conditions for 48 hours. After the reaction was completed, it was naturally cooled to room temperature. Take it out and dry it in a drying oven at 45°C to obtain a one-dimensional linear full-color nano-fluorescent powder with a diameter of about 10-80 nm and a length of 30-1000 microns.

Embodiment 3

[0052] Embodiment 3. 1.046g GeO 2 , 0.3976g CaO, 0.8018g europium acetate tetrahydrate, 0.453g terbium nitrate hexahydrate mixed with 120ml deionized water, after ultrasonic treatment for 30min, moved into a 200ml polytetrafluoroethylene reactor, placed in a heating furnace, at 160 ℃ temperature conditions for 24 hours. After the reaction was completed, it was naturally cooled to room temperature. Take it out and dry it in a drying oven at 60°C to obtain a one-dimensional linear full-color nano-phosphor powder with a diameter of about 10-80 nm and a length of 30-1000 microns.

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Abstract

The invention provides a preparation method of blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder, belonging to the field of a luminescent material preparation technology. The preparation method comprises the following steps: weighing raw materials according to the chemical mole component match ratio is determined by the general chemical formula of the panchromatic nanofluorescent powder: R (1-a-b) GewOu: aEu<3+>, bTb<3+> or MzR (1-x-y-z) GewOu: xEu<3+>, yTb<3+>, wherein R is one of Ca, Sr and Ba, and M is at least one of Li, Na and K; adding the raw materials into water to carry out ultrasonic treatment for 30-60 minutes and then transferring the treated raw materials into a reaction kettle, wherein the filling degree of a reaction kettle is controlled as 60-85%; carrying out heat preservation on the raw materials for 1-48 hours at the temperature of 100-200 DEG C, cooling and filtering; and drying filter residues at a temperature of 60-90 DEG C, so as to obtain the one-dimensional panchromatic nanofluorescent powder. The preparation method of the blue-light and near ultraviolet excitation type one-dimensional panchromatic nanofluorescent powder provided by the invention is simple, safe and controllable in technology, low in preparation temperature, low in energy consumption and uniform in component distribution, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a blue-light and near-ultraviolet excited one-dimensional full-color nano-fluorescent powder, which belongs to the technical field of luminescent material preparation. Background technique [0002] Solid-state lighting is a technology that uses semiconductor light-emitting diodes (LEDs) to manufacture lighting sources. It has significant advantages such as green environmental protection, good weather resistance, high theoretical light efficiency, energy saving, long life, rich colors, fast response, easy miniaturization and maintenance-free. , so it is known as a new generation of light sources after incandescent lamps, fluorescent lamps and energy-saving lamps. It is expected to replace traditional lighting sources and has very broad application prospects. Based on the current development of LED technology and production costs, the way to obtain white LEDs is mainly to use near-ultraviolet or blue LED s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66
Inventor 林良武江垚贺跃辉
Owner CENT SOUTH UNIV