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Preparation method for nitride fluorescent powder and equipment for same

A nitride phosphor and phosphor technology, applied in chemical instruments and methods, chemical industry, luminescent materials, etc., can solve the problem of reducing the luminous intensity and thermal stability of products, affecting the luminous efficiency of nitride phosphors, and unable to achieve large-scale production. Stable preparation of nitride phosphors, etc., to achieve the effect of ensuring safety and service life, good luminous performance, and high nitrogen-containing purity

Inactive Publication Date: 2015-01-14
湖南爱德光电新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the patent mentions the synthesis of high-efficiency nitride phosphors, there is a problem of how to remove excess carbon in the synthesis of nitride phosphors by carbon reduction, and the insufficient reducing atmosphere makes doped Eu coexist in divalent and trivalent. The patent does not mention how to solve it, and this problem will directly affect the luminous efficiency of nitride phosphors; another example: patent application 200910147787.3, using oxide nitriding as a raw material method, adopting a high-temperature solid-phase method at 1300°C-1800°C Preparation of nitride phosphor M at ℃ 2-w Si x A y N z : w R (R=Eu, Sm, Ce) red phosphor, oxide nitriding can avoid the problem of easy oxidation of raw materials, but the use of oxide raw materials will cause a large amount of lattice oxygen to exist in the product, reducing the luminous intensity and thermal stability of the product Another example: patent application 201010602118.3, using a high-temperature solid-phase method to prepare nitride phosphors at 1350-2000 ° C and 5-200 atmospheres. powder to meet market demand for nitride phosphors

Method used

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  • Preparation method for nitride fluorescent powder and equipment for same
  • Preparation method for nitride fluorescent powder and equipment for same
  • Preparation method for nitride fluorescent powder and equipment for same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Use the equipment of the invention to prepare nitride red phosphor Sr 1.98 Si 5 N 8 : 02 Eu. Before the operation starts, such as figure 1 , Various equipment and gates are in the closed state, the specific operations are as follows:

[0034] (1) Pass the raw materials into the glove box through the first transition chamber, open the raw material tank in the glove box, and weigh the corresponding weight of Si according to the stoichiometric ratio 3 N 4 , Sr 2 N 3 And Eu 2 N 3 Raw material, BaF with a mass fraction of 0.01% 2 As a fluxing agent, it is uniformly mixed with the mixing device for 12 hours and then taken out, and filled in a 100mL graphite crucible. The above process is carried out in a glove box, and the glove box is filled with 1.0 atmosphere of nitrogen as a protective atmosphere;

[0035] (2) Place the graphite crucible filled with the sample in the transfer device through the second transition chamber, enter the third transition chamber and the fourth transit...

Embodiment 2

[0039] Use the equipment of the invention to prepare nitride red phosphor Ca 0.3 Sr 1.5 Si 5 N 8 : 0.2 Eu. Before the operation starts, such as figure 1 , Various equipment and gates are in the closed state, the specific operations are as follows:

[0040] (1) Pass the raw materials into the glove box through the first transition compartment, open the raw material tank in the glove box, and weigh the corresponding weight of Ca according to the stoichiometric ratio 2 N 3 , Si 3 N 4 , Sr 2 N 3 And Eu 2 N 3 The raw material, BaF2 with a mass fraction of 5% as a flux, is uniformly mixed in the mixing device for 24 hours and then taken out, and filled in a 100mL graphite crucible. The above process is carried out in a glove box, and the glove box is filled with 1.5 atmospheres of nitrogen as Protective atmosphere

[0041] (2) Place the graphite crucible filled with the sample in the conveying device through the second transition chamber, enter the third transition chamber and the fourth...

Embodiment 3

[0045] Adjust red phosphor raw material Ca 2 N 3 And Sr 2 N 3 The ratio of stoichiometry meets Ca 0.6 Sr 1.2 Si 5 N 8 : 0.2 Eu, Ca 0.9 Sr 0.9 Si 5 N 8 : 0.2 Eu, other steps are the same as in Example 2, and the emission spectrum of the sample is shown in the attachment Figure 7-3 And Figure 7-4 , It can be clearly found that with the increase in the proportion of Ca and the decrease of the proportion of Sr, the emission peak of the sample moves in the direction of Zhang long wave.

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Abstract

The invention discloses a method for preparing a nitride fluorescent powder by a high-temperature solid-phase method, and production equipment used for the method. The method comprises the following steps of: (1) detaching raw materials in an oxygen-free and water-free glove box, and mixing the raw materials in a mixing device arranged in the glove box; (2) transferring the mixed raw materials to a reduction furnace via a transition device under nitrogen protection, and solving the problems of other backflows and isolated heat transfer via a transition cabin; (3) calcining at a high temperature in a nitrogen / hydrogen atmosphere by adopting a subsection temperature control method in which three parts, a preheating area, a high-temperature area and a cooling area are formed; and (4) performing aftertreatment on the cooled sample in room-temperature air. By using the method and the equipment, the high-purity nitride fluorescent powder can be manufactured, and the central granularity of the fluorescent powder and the position of an emitting main peak can be controlled by adjusting the calcining temperature and the composition ratio of the raw materials respectively; and with the adoption of three-section calcining, preparation for the nitride fluorescent powder by the method can realize continuous production, thus greatly increasing production efficiency. The method is energy-saving, environment-friendly, and suitable for mass preparation for the nitride fluorescent powder.

Description

Technical field: [0001] The invention belongs to the field of luminescent material and equipment manufacturing, and particularly relates to a method for preparing nitride phosphors and manufacturing equipment thereof. Background technique: [0002] Light-emitting diodes (LEDs) are new solid-state lighting devices developed in recent years, which have the advantages of high efficiency, long life, no pollution, and energy saving. Countries around the world have invested a lot of manpower and financial resources in the research and development of white LEDs. At present, commercial white LEDs generally use the combination of blue chip + yellow phosphor YAG:Ce. This combination has high luminous efficiency. The disadvantage is that it lacks red light radiation, low color rendering index, high color temperature, and the oxide phosphor itself is hot. The stability is poor and cannot meet the requirements of high-power white light LEDs. Nitride red phosphor M 2 Si 5 N 8 : Eu (M=Ca, Sr,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64C09K11/59
CPCY02P20/10
Inventor 周智刘素琴蒋葵明曾少波刘清玲
Owner 湖南爱德光电新材料有限公司
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