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A kind of yb for white light led 2+ Excited nitrogen oxide green fluorescent material and preparation method thereof

A green fluorescence and nitrogen oxide technology, which is applied in the direction of luminescent materials, chemical instruments and methods, electrical components, etc., can solve the problems of inapplicable nitrogen oxide stable production, unsuitable for market-oriented batch production, and affecting the commercialization process, etc. , to achieve the effects of large-scale production, green and environmentally friendly synthesis process, and short preparation cycle

Active Publication Date: 2020-07-14
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of nitrogen oxide fluorescent materials usually requires the use of alkaline earth metal nitrides or high-purity metal powders as matrix materials, and many of them also use rare earth nitrides as doping materials. 2 It is extremely sensitive to moisture and moisture, so it must be operated in a vacuum glove box or a pure nitrogen glove box, otherwise it is easy to be oxidized and has the possibility of explosion, so it is not suitable for mass production in the market
However, cheap alkaline earth metal carbonates are not suitable for the stable production of nitrogen oxides because of their oxygen content, which can cause unpredictable damage to the nitriding process.
[0004] As an essential raw material for the preparation of silicon-based oxynitride, Si 3 N 4 The powder has a strong covalent bond, resulting in low diffusion coefficient and poor reactivity. Therefore, a high synthesis temperature is required in the preparation process of silicon-based oxynitride, and high-pressure nitrogen gas needs to be introduced to inhibit its decomposition, which leads to A substantial increase in production costs seriously affected the process of its commercialization
In the past, the activator used to obtain green light was mainly Eu 2+ and Tb 3+ , both of which have small absorption cross section and high price

Method used

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  • A kind of yb for white light led  <sup>2+</sup> Excited nitrogen oxide green fluorescent material and preparation method thereof
  • A kind of yb for white light led  <sup>2+</sup> Excited nitrogen oxide green fluorescent material and preparation method thereof
  • A kind of yb for white light led  <sup>2+</sup> Excited nitrogen oxide green fluorescent material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] According to the chemical molar ratio of 2.985:2:0.0075, accurately weigh 0.39835g CaCO 3 , 0.30674g NH 4 h 2 PO 4 and 0.00394g Yb 2 o 3 , mix the raw materials and add 1 mL of ethanol for trituration. After grinding evenly, add high-purity Al 2 o 3 The crucible was sintered in a tube furnace at 1200 °C for 2 h, cooled to room temperature and ground to obtain the precursor Ca 3-x (PO 4 ) 2 : 2x / 3Yb 3 + (x=0.01). The resulting precursor and 0.41333g Si 3 N 4 The powders were mixed, then put into an agate mortar and 1mL of ethanol was added for thorough grinding. The mixture obtained after grinding and drying was put into a high-purity graphite ark, kept and sintered in a high-temperature tube furnace at 1400 ° C for 5 h, and the gas flow rate was 400 mL / min. 2 / H 2 mixed gas. The nitrogen oxide green fluorescent material is obtained by grinding after being cooled to room temperature in the furnace.

Embodiment 2

[0039] According to the chemical molar ratio of 2.97:2:0.015, accurately weigh 0.39636g CaCO 3 , 0.30674g NH 4 h 2 PO 4 and 0.00788g Yb 2 o 3 , mix the raw materials and add 1 mL of ethanol for trituration. After grinding evenly, add high-purity Al 2 o 3 The crucible was sintered in a tube furnace at 1200 °C for 2 h, cooled to room temperature and ground to obtain the precursor Ca 3-x (PO 4 ) 2 : 2x / 3Yb 3+ (x=0.02). The resulting precursor and 0.41333g Si 3 N 4 The powders were mixed, then put into an agate mortar and 1mL of ethanol was added for thorough grinding. The mixture obtained after grinding and drying was put into a high-purity graphite ark, kept and sintered in a high-temperature tube furnace at 1400 ° C for 5 h, and the gas flow rate was 400 mL / min. 2 / H 2 mixed gas. The nitrogen oxide green fluorescent material is obtained by grinding after being cooled to room temperature in the furnace.

Embodiment 3

[0041] According to the chemical molar ratio (2.955): 2:0.0225, accurately weigh 0.39435g CaCO 3 , 0.30674gNH 4 h 2 PO 4 and 0.01182g Yb 2 o 3 , mix the raw materials and add 1 mL of ethanol for trituration. After grinding evenly, add high-purity Al 2 o 3 The crucible was sintered in a tube furnace at 1200 °C for 2 h, cooled to room temperature and ground to obtain the precursor Ca 3-x (PO 4 ) 2 :2x / 3Yb 3+ (x=0.03). The resulting precursor and 0.41333g Si 3 N 4 The powders were mixed, then put into an agate mortar and 1mL of ethanol was added for thorough grinding. The mixture obtained after grinding and drying was put into a high-purity graphite ark, kept and sintered in a high-temperature tube furnace at 1400 ° C for 5 h, and the gas flow rate was 400 mL / min. 2 / H 2 mixed gas. The nitrogen oxide green fluorescent material is obtained by grinding after being cooled to room temperature in the furnace.

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Abstract

The invention relates to the technical field of rare-earth light emitting materials and in particular discloses a Yb<2+> excited nitric oxide green fluorescent material for a white light LED (light emitting diode) and a preparation method of the fluorescent material. The fluorescent material has a chemical expression formula of Ca2-xSi3O2N4: xYb<2+>, and in the formula, x is greater than or equalto 0.01 and less than or equal to 0.06. The preparation method comprises the following steps: accurately weighing CaCO3, NH4H2PO4 and Yb2O3 according to a chemical mole ratio; obtaining a precursor Ca3-x(PO4)2: xYb<3+> through mixing, grinding, and high-temperature sintering; mixing and grinding the precursor with Si3N4, carrying out high-temperature sintering, and introducing an N2 / H2 mixed gas,thereby obtaining the fluorescent material. The fluorescent material provided by the invention has excellent light emission properties, has effective broadband absorption from an ultraviolet region toa blue light region, is matched with a chip of a commercial LED, and has an emission wave peak at 545nm. The fluorescent material is short in preparation cycle, simple in process procedure, low in equipment requirement, green and environmentally-friendly in synthesis process and beneficial to large-scale production.

Description

technical field [0001] The invention belongs to the technical field of rare earth luminescent materials, in particular to Yb for white light LEDs 2+ Excited nitrogen oxide green fluorescent material and preparation method thereof. Background technique [0002] White light LED is a new generation of green lighting source, and its white light is mainly emitted by phosphor conversion method. Traditional oxide, sulfide, and halide system phosphors have poor stability and unstable chemical properties, while borate, silicate, and aluminate system phosphors have stable chemical properties, but have a single structure and single spectral properties, making it difficult to Match with specific LED chips. Therefore, nitrogen oxide fluorescent materials with stable physical and chemical properties, rich spectral properties and environmental friendliness have received extensive attention since their inception. [0003] At present, the preparation of nitrogen oxide fluorescent material...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59H01L33/50
CPCC09K11/77H01L33/502Y02B20/00
Inventor 于立新邹颖璇高震宇
Owner NANCHANG UNIV
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