Fluorosilicate-based up-conversion luminescent ceramic material and preparation method thereof

A technology of luminescent ceramics and fluorosilicate, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of complex preparation process, insufficient stability, the use and popularization and application of up-conversion luminescent materials, etc., and achieve good repeatability , Improve the excitation stability, and the effect of rich raw material sources

Active Publication Date: 2019-01-11
NANJING TONGLI CRYSTAL MATERIALS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, up-conversion luminescent materials are mainly concentrated in rare earth-doped fluoride, sulfide, halide and other systems, which can realize the emission of red, green, blue and white light. However, in practical applications, due to the insufficient stability of these matrix materials, The preparation process is complex, which has a great impact on the use and promotion of up-conversion luminescent materials

Method used

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  • Fluorosilicate-based up-conversion luminescent ceramic material and preparation method thereof
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  • Fluorosilicate-based up-conversion luminescent ceramic material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0027] Preparation of Ca 9.45 Er 0.05 Yb 0.5 Si 3 o 15 f 2 , according to the chemical formula Ca 9.45 Er 0.05 Yb 0.5 Si 3 o 15 f 2 The stoichiometric ratio of each element in, weighed calcium carbonate CaCO 3 : 8.503 g, silicon oxide SiO 2 : 1.8024 g, erbium oxide Er 2 o 3 : 0.0010 g, ytterbium oxide Yb 2 o 3 : 0.010 g, ground and mixed uniformly in an agate mortar, pre-sintered in an air atmosphere, the sintering temperature is 800 ° C, the sintering time is 10 hours, then cooled to room temperature, the sample is taken out and ground and mixed uniformly; the pre-sintered mixture is mixed with 0.7808 g calcium fluoride CaF 2Thoroughly mix and grind evenly, and press the mixed powder with a pressing pressure of 10 MPa, then calcinate again in an air atmosphere, calcining temperature is 1100°C, calcining time is 5 hours, naturally cool, grind and mix uniformly to obtain calcium fluorosilicate fluorescent ceramics.

[0028] See attached figure 1 , which is the...

Embodiment 2

[0032] Preparation of Ca 9.49 Er 0.01 Yb 0.5 Si 3 o 15 f 2 , according to the chemical formula Ca 9.49 Er 0.01 Yb 0.5 Si 3 o 15 f 2 The stoichiometric ratio of each element in , respectively weigh calcium hydroxide Ca(OH) 2 : 4.9648 g, silicic acid H 2 SiO 3 : 2.34 g, erbium oxide Er 2 o 3 : 0.0020 g, ytterbium oxide Yb 2 o 3 : 0.010 g, ground and mixed uniformly in an agate mortar, pre-sintered in an air atmosphere, the sintering temperature is 950 ° C, the sintering time is 3 hours, then cooled to room temperature, the sample is taken out and ground and mixed uniformly; the pre-sintered raw material is mixed with 2.3424 grams of calcium fluoride CaF 2 Thoroughly mix and grind evenly, and press the mixed powder with a pressing pressure of 15 MPa, then calcinate again in an air atmosphere, calcining temperature is 950°C, calcining time is 10 hours, naturally cool, grind and mix evenly to obtain calcium fluorosilicate fluorescent ceramics.

[0033] The X-ray p...

Embodiment 3

[0035] Preparation of Ca 9.4 Er 0.1 Yb 0.5 Si 3 o 15 f 2 , according to the chemical formula Ca 9.4 Er 0.1 Yb 0.5 Si 3 o 15 f 2 The stoichiometric ratio of each element in , respectively weigh calcium oxalate CaC 2 o 4 : 9.507 g, silicic acid H 2 SiO 3 : 2.34 g, erbium oxide Er 2 o 3 : 0.020 g, ytterbium oxide Yb 2 o 3 : 0.010 g, ground and mixed in an agate mortar, pre-sintered in an air atmosphere, the sintering temperature is 900 ° C, the sintering time is 4 hours, then cooled to room temperature, the sample is taken out and ground and mixed evenly; the pre-sintered raw materials are again with 1.5616 g of calcium fluoride CaF 2 Thoroughly mix and grind evenly, and press the mixed powder into shape, the pressing pressure is 12MPa, calcined again in the air atmosphere, the calcining temperature is 900°C, the calcining time is 15 hours, the natural cooling is ground and mixed evenly to obtain calcium fluorosilicate fluorescent ceramics.

[0036] The X-ray p...

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Abstract

The invention discloses a fluosilicate based up-conversion luminescence ceramic material and a preparation method thereof; the general chemical formula of the ceramic material is Ca10-10xEr10xYb10ySi3O15F2, wherein x is Er3+ doped chemical metering percent, y is ytterbium ion Yb+3 mixed chemical metering percent, 0.001 is not more than x+y< 0.2. The up-conversion luminescence ceramic material prepared by the method is stable in crystal structure, uniform in grain diameter size, and stable in lighting performance; under the excitation of 976 nanometer infrared laser, a red lighting peak is appeared in the vicinity of 670 nanometer, and the lighting purity is high, and the up-conversion efficiency is high. For the matrix structure is stable and the doped rare earth concentration is high, the ceramic material is good for enhancing the lighting efficiency and realizing the excitation under a high power. In preparation, the compounds containing elements required by compounding lighting materials are mixed at ratio, the ceramic material is prepared by a high-temperature solid phase method; the preparation method is simple in technique, rich in raw material source, and low in price; moreover, the technique process is free from waste water and waste gas, and is toxic-free and environment-friendly; the fluosilicate based up-conversion luminescence ceramic material is further popularized and used.

Description

technical field [0001] The invention relates to the field of solid fluorescent materials, in particular to a fluorosilicate-based up-conversion luminescent ceramic material and a preparation method thereof. Background technique [0002] In recent years, upconversion luminescent materials have attracted extensive attention. Among photoluminescent materials, the luminescent materials that absorb two or more photons of lower energy and emit one high-energy photon are defined as up-conversion luminescent materials (UCPs for short). The essence of the upconversion phenomenon of this material is the anti-Stokes effect, that is, the radiated energy is greater than the absorbed energy. The principle of light emission is that when the light source shines on the surface of the material, the particles will absorb two or more low-energy excitation photons. , the electrons transition from the ground state to a high-energy state, and then radiate high-energy photons outward, and the freq...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/86C04B35/16C04B35/622
CPCC04B35/16C04B35/622C04B2235/3208C04B2235/3224C04B2235/445C09K11/7774
Inventor 乔学斌
Owner NANJING TONGLI CRYSTAL MATERIALS RES INST CO LTD
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