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Organic-inorganic hybrid fluorine titanium potassium red-light fluorescent powder and preparation method thereof

A technology of red fluorescent powder and hybridization, applied in chemical instruments and methods, luminescent materials, electrical components, etc., can solve the problems of poor moisture resistance, decreased luminous intensity, no luminescence, etc., and achieve high luminescence with low requirements for reaction conditions Thermal stability, the effect of simple preparation method

Active Publication Date: 2022-03-15
广西经正涂料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But existing Mn 4+ Doped fluoride red phosphors also have some disadvantages to overcome: (1) The luminous intensity is higher than that of yellow phosphors YAG:Ce 3+ The weight ratio of it to yellow light powder is as high as 2:1-3:1 during application; (2) The thermal stability is not high, and the luminous intensity is often caused by thermal quenching at the working temperature of white LEDs (about 150°C). extinguished and dropped to 70-80% of the original; (3) poor moisture resistance, in humid environment, Mn 4+ Easily hydrolyzed into opaque MnO 2 , and then rapidly deactivate without emitting light

Method used

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  • Organic-inorganic hybrid fluorine titanium potassium red-light fluorescent powder and preparation method thereof
  • Organic-inorganic hybrid fluorine titanium potassium red-light fluorescent powder and preparation method thereof
  • Organic-inorganic hybrid fluorine titanium potassium red-light fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Preparation [KTF:0.06Mn 4+ ,0.10tetaH + ]

[0036] (1) First, under stirring, add 1.4623g (10mmol) of tetra dropwise to 48.01g (100mmol) of 50% H 2 TiF 6 H in solution 2 TiF 6 -tetaH + Mix the solution, then add 11.06g (80.0mmol) K 2 CO 3 Added to 30mL of deionized water, stirred until completely dissolved to obtain K 2 CO 3 solution; then, under stirring, the K 2 CO 3 The solution was added dropwise to the above H 2 TiF 6 -tetaH + After dripping the mixed solution until the pH is 7.0, continue to stir for 30 minutes, then seal the mouth of the beaker with plastic wrap and place it in an oven at 90°C for 3 hours; finally remove the plastic wrap and place it in an oven at 120°C Under drying for 4h, to obtain the intermediate K 2 TiF 6 :0.10tetaH + ;

[0037] (2) get 12.39mLHF solution (mass concentration 40%) (V HF / W 基质 =3.0mL / g), 0.413g KF·2H 2 O(W KF / W 基质 =0.1), 0.2966g (1.2mmol) K 2 MnF 6 The powder is placed in a 50mL plastic ...

Embodiment 2

[0046] Embodiment 2: preparation [KTF:0.01Mn 4+ ,0.02tetaH + ]

[0047] (1) First, under stirring, add 0.2925g (2mmol) of tetra dropwise to 48.01g (100mmol) of 50% H 2 TiF 6 H in solution 2 TiF 6 -tetaH + Mix the solution, then add 13.27g (96.0mmol) K 2 CO 3 Add 30mL of deionized water and stir until completely dissolved to obtain K 2 CO 3 solution; then, under stirring, the K 2 CO 3 The solution was added dropwise to the above H 2 TiF 6 -tetaH + After dropping the mixed solution until the pH is 7.0, continue to stir for 20 minutes, then seal the mouth of the beaker with a plastic wrap and place it in an oven for 3.5 hours at 85°C; finally remove the plastic wrap and place it in an oven at 130°C Dry at ℃ for 3h, to obtain intermediate K 2 TiF 6 :0.02tetaH + ;

[0048] (2) get 4.4mLHF solution (mass concentration 40%) (VHF / W 基质 =1.0mL / g), 0.872g KF·2H 2 O(W KF / W 基质 =0.2), 0.0494g (0.2mmol) K 2 MnF 6 The powder is placed in a 50mL plastic beaker, stirre...

Embodiment 3

[0051] Embodiment 3: preparation [KTF:0.02Mn 4+ ,0.06tetaH + ]

[0052] (1) First, under stirring, add 0.8774g (6mmol) of tetra dropwise to 48.01g (100mmol) of 50% H 2 TiF 6 H in solution 2 TiF 6 -tetaH + Mix the solution, then put 12.16g (88.0mmol) K 2 CO 3 Add 30mL of deionized water and stir until completely dissolved to obtain K 2 CO 3 solution; then, under stirring, the K 2 CO 3 The solution was added dropwise to the above H 2 TiF 6 -tetaH + After dropping the mixed solution until the pH is 7.0, continue stirring for 25 minutes, then seal the mouth of the beaker with plastic wrap and place it in an oven at 95°C for 4 hours; finally remove the plastic wrap and place it in an oven at 130°C Under drying for 3.5h, intermediate K was obtained 2 TiF 6 :0.06tetaH + ;

[0053] (2) Take 19.63mL HF solution (mass concentration 40%) (V HF / W 基质 =4.0mL / g), 1.4723g KF 2H 2 O(W KF / W 基质 =0.3), 0.0989g (0.4mmol) K 2 MnF 6 The powder is placed in a 50mL plastic b...

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Abstract

The invention belongs to the technical field of preparation of fluorescent powder, and particularly relates to organic-inorganic hybrid fluorine titanium potassium red-light fluorescent powder, the general formula of which is K2TiF6: xMn < 4 + >, ytetaH < + >, tetaH < + > represents that triethylene tetramine is subjected to organic-inorganic hybridization, and triethylene tetramine exists in a protonation form after hybridization; x is the mole fraction of Mn < 4 + > doping, y is the mole fraction of triethylene tetramine doping, x is larger than or equal to 0.01 and smaller than or equal to 0.12, and y is larger than or equal to 0.0 and smaller than or equal to 0.15. The invention also provides a preparation method of the organic-inorganic hybrid potassium titanium fluoride red-light fluorescent powder, which comprises the following steps: (1) reacting triethylene tetramine with an H2TiF6 solution and a K2CO3 solution, and drying to obtain K2TiF6: ytetaH < + >; and (2) reacting KF. 2H2O with an HF solution, a K2MnF6 solution and K2TiF6: ytetaH < + >, sealing, standing, carrying out suction filtration, washing and drying to obtain the K2TiF6: xMn < 4 + >, ytetaH < + >. The obtained red-light fluorescent powder has the advantages of high luminescence, high intensity, water resistance, thermal stability and the like.

Description

technical field [0001] The invention belongs to the technical field of fluorescent powder preparation, and in particular relates to an organic-inorganic hybrid fluorine-titanium-potassium red-light fluorescent powder. Background technique [0002] Diodes (white LEDs) have the advantages of high luminous efficiency, energy saving, long life, low energy consumption, and environmental protection. Therefore, LEDs are regarded as a new generation of solid-state light-emitting devices. At present, the most mature and commercialized white LEDs are based on blue chip and yellow phosphor YAG:Ce 3+ Realized by the combination of yellow light phosphor YAG:Ce 3+ Absorption of the blue light emitted by the blue chip produces yellow fluorescence, which is combined with the chip's blue light to obtain white light. Because this kind of white light lacks red light components, it has disadvantages such as high color temperature and low color purity, so it is difficult to apply to general l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/67C09K11/06H01L33/50
CPCC09K11/675C09K11/06H01L33/504C09K2211/188Y02B20/00
Inventor 黄映恒廖森黄毅于艳强嘉伟李燕石云浩
Owner 广西经正涂料有限公司
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