CN102031109A - Single-phase white light fluorescent powder based on near-UV excitation and preparation method thereof - Google Patents

Abstract

The invention belongs to the field of luminescent materials, and discloses single-phase white light fluorescent powder based on near-UV excitation. The molecular formula of the single-phase white light fluorescent powder is LiCa3SrMgV3O12:Eu<3+>. In the preparation method of the fluorescent powder, the following materials are weighed by weight: 30-40g of Li2CO3, 275-290g of CaCO3, 25-35g of SrCO3, 340-360g of NH4VO3, 35-45g of MgO, and 8-16g of Eu2O3, wherein the weight percentages of the materials are as follow: 4-7% of Li2CO3, 32-40% of CaCO3, 2-6% of SrCO3, 40-50% of NH4VO3, 4-7% of MgO and 1-5% of Eu2O3, and the preferable weight ratio of Li2CO3 to CaCO3 to SrCO3 to NH4VO3 to MgO to Eu2O3 is 0.05:0.38:0.04:0.47:0.04:0.015; and 0.2-0.5% of a fluxing agent BaF2 or H3BO3 is added; and the preparation method is a high temperature solid-phase method. The single-phase white light fluorescent powder can be efficiently excited by near UV of 365nm to respectively present two emission spectrums of 530nm and 610nm so that efficient white light is emitted. Therefore, the fluorescent powder has the advantages of good stability and high luminous intensity.

Description

A kind of near ultraviolet excitation single-phase white-emitting phosphor and preparation method thereof

Technical field

The invention belongs to field of light emitting materials, particularly a kind of near ultraviolet excitation single-phase white-emitting phosphor and preparation method thereof.

Background technology

The technology of producing white light LEDs mainly contains two kinds at present, and the one, utilize super brightness In-GaN blue led, add on its tube core that the yttrium aluminum garnet (YAG) of a little is the fluorescent material of main body.In-GaN chip blue light-emitting, YAG fluorescent material sends sodium yellow after being subjected to this blue-light excited.The blue light that chip appears is in the same place with the yellow light mix of fluorescent material, forms white light; The 2nd, the principle of three primary colours and three kinds of ultra-high brightness LEDs of fertile at present red, green, blue form white by 1: 2: 0.38 mixed of light intensity.

First kind of its white light is to be formed by the yellow fluorescence of luminescent powder and the blue light of led chip, stability better, but too low about 82 of its luminous more dazzling, colour rendering index is to showing that the high occasion of object color can't use.

And second kind of employing near-ultraviolet light InGaN tube core excites the red, green, blue three primary colors fluorescent powder to realize that white light LEDs is better than first kind.Because near-ultraviolet light is invisible to naked eyes, the color of this class white light LEDs is only determined by fluorescent material.If yet adopt heterogeneous fluorescent material to realize white light, will exist color to absorb again and proportioning regulation and control problem between the phosphor mixture, luminous efficiency and color rendition performance are a greater impact.

Also have a kind of method to adopt near-ultraviolet light InGaN tube core to excite a kind of single-matrix white fluorescent powder to realize white light, because this white fluorescent powder mainly contains the red emission band that main peak is positioned at the bluish-green emission band of 520nm and is positioned at 616nm under near ultraviolet excitated, directly emit white light, do not need three kinds of fluorescent material of red, green, blue to mix just and can emit white light, because it is that two emission peaks are arranged in a kind of fluorescent material, can directly emit white light, just there are not top two kinds of these problems, and two kinds advantage all possesses.

Summary of the invention

The purpose of this invention is to provide a kind of near ultraviolet excitation single-phase white-emitting phosphor;

Another object of the present invention provides a kind of preparation method of near ultraviolet excitation single-phase white-emitting phosphor.

The molecular formula of near ultraviolet excitation single-phase white-emitting phosphor of the present invention is: LiCa ₃SrMgV ₃O ₁₂: Eu ³⁺The preparation method of near ultraviolet excitation single-phase white-emitting phosphor of the present invention may further comprise the steps:

(1) takes by weighing Li ₂CO ₃30-40g, CaCO ₃275-290g, SrCO ₃25-35g, NH ₄VO ₃340-360g, MgO35-45g, Eu ₂O ₃8-16g adds the fusing assistant BaF of 0.2-0.5% ₂Or H ₃BO ₃Each raw material weight ratio is: Li ₂CO ₃4-7%, CaCO ₃32-40%, SrCO ₃2-6%, NH ₄VO ₃40-50%, MgO 4-7%, Eu ₂O ₃1-5%; Obtain mixture and mix;

(2) mixed raw material is put into 700-1000 ℃ of calcination of aire tunnel kiln 2～4 hours, taken out and be cooled to room temperature, obtain work in-process, indexs such as test relative brightness, emission main peak, granularity;

(3) work in-process are pulverized, scalping washing, wet screening, centrifugal, dried 100 mesh sieves, the test synthesis data obtain finished product.

The preparation of near ultraviolet excitation single-phase white-emitting phosphor of the present invention, each raw material preferred weight ratio is Li ₂CO ₃:, CaCO ₃: SrCO ₃: NH ₄VO ₃: MgO: Eu ₂O ₃=0.05: 0.38: 0.04: 0.47: 0.04: 0.015.

Near ultraviolet excitation single-phase white-emitting phosphor of the present invention can present two emmission spectrum efficiently by the 365nm near ultraviolet excitation, is respectively 530nm, 610nm, sends efficient white light, good stability, luminous intensity height.Preparation technology is simple, be easy to industrialization, therefore near ultraviolet excitation single-phase white-emitting phosphor of the present invention can with near-ultraviolet light tube core combined preparation white light LEDs, to overcome present red, green, blue three primary colours mixed fluorescent powder because of absorbing again of existing with proportioning is regulated and control the defective that problem influences luminous efficiency and color rendition performance.

Embodiment

Below the present invention is done a detailed description

(4) molecular formula of near ultraviolet excitation single-phase white-emitting phosphor is:: LiCa ₃SrMgV ₃O ₁₂: Eu ³⁺Take by weighing Li ₂CO ₃30-40g, CaCO ₃275-290g, SrCO ₃25-35g, NH ₄VO ₃340-360g, MgO35-45g, Eu ₂O ₃8-16g adds the fusing assistant BaF of 0.2-0.5% ₂Or H ₃BO ₃Each raw material weight ratio is: Li ₂CO ₃4-7%, CaCO ₃32-40%, SrCO ₃2-6%, NH ₄VO ₃40-50%, MgO 4-7%, Eu ₂O ₃1-5%; Obtain mixture and mix; 700-1000 ℃ of calcination 2～4 hours, taking-up is cooled to room temperature, obtain work in-process, indexs such as test relative brightness, emission main peak, granularity obtain work in-process and test indexs such as relative brightness, emission main peak, granularity, with work in-process pulverize, scalping washing, wet screening, centrifugal, dried 100 mesh sieves, the test synthesis data obtain finished product.Present two emmission spectrum with the test of fluorescence spectrum tester, be respectively 530nm, 610nm.

The preparation of near ultraviolet excitation single-phase white-emitting phosphor of the present invention, each raw material preferred weight ratio is Li ₂CO ₃:, CaCO ₃: SrCO ₃: NH ₄VO ₃: MgO: Eu ₂O ₃=0.05: 0.38: 0.04: 0.47: 0.04: 0.015.

Claims (2)

1. near ultraviolet excitation single-phase white-emitting phosphor, it is characterized in that: the molecule of near ultraviolet excitation single-phase white-emitting phosphor is: LiCa ₃SrMgV ₃O ₁₂: Eu ³⁺

2. the preparation method of near ultraviolet excitation single-phase white-emitting phosphor according to claim 1 is characterized in that: described method steps comprises:

(1) takes by weighing Li ₂CO ₃30-40g, CaCO ₃275-290g, SrCO ₃25g-35, NH ₄VO ₃340g-360, MgO35-45g, Eu ₂O ₃8-16g adds the fusing assistant BaF of 0.2-0.5% ₂Or H ₃BO ₃Each raw material weight ratio is: Li ₂CO ₃4-7%, CaCO ₃32-40%, SrCO ₃2-6%, NH ₄VO ₃40-50%, MgO 4-7%, Eu ₂O ₃1-5%; Obtain mixture and mix;

(2) mixed raw material is put into 700-1000 ℃ of calcination of aire tunnel kiln 2～4 hours, taken out and be cooled to room temperature, obtain work in-process, indexs such as test relative brightness, emission main peak, granularity;

(3) work in-process are pulverized, scalping washing, wet screening, centrifugal, dried 100 mesh sieves, the test synthesis data obtain finished product.