CN107141805A - A kind of flexible red fluorescence film - Google Patents

Abstract

The invention discloses a flexible red fluorescent film, which is composed of powder and organic matter, the mass ratio of powder and organic matter is (0.1-0.3):1, and the organic matter is polydimethylsiloxane. In the powder, based on the mass percentage of oxides, the total content of 0%<Na ₂ O+Li ₂ O+K ₂ O<6.65%, 0<MgO<8.65%, 30%<WO ₃ +MoO ₃ The total content <49.75%, the total content of 5%<Gd ₂ O ₃ +La ₂ O ₃ +Y ₂ O ₃ <34.95%, 0%<Eu ₂ O ₃ <22.28%. The present invention also provides a preparation method for the above-mentioned flexible red fluorescent film, which is simple in operation and low in cost, can improve the consistency of phosphor coating and heat dissipation, and is suitable for remote phosphor LED packaging and large-scale and batch industrialization Production.

Description

A flexible red fluorescent film

technical field

The invention belongs to the field of material science and relates to a fluorescent film, in particular to a flexible red fluorescent film.

Background technique

Because white LED devices have the advantages of high luminous efficiency, low power consumption and environmental friendliness, white light emitting diodes (LEDs) have attracted much attention in recent years. Because the phosphor is granular, it is easy to agglomerate on the substrate, and the adhesion to the substrate is also poor, and the thermal stability and uniformity are not good. Due to its good thermal stability, uniformity, and good adhesion to the substrate, fluorescent thin films have recently received more and more attention. The traditional dispensing method is not conducive to the heat dissipation of the LED chip, resulting in uneven white light and serious scattering. Because the fluorescent film is beneficial to the array packaging and heat dissipation of LED chips, it has become a research hotspot in recent years.

The flexible red fluorescent film made of remote red phosphor can be used in high-power LED lamps, avoiding the direct contact between the phosphor material and the energy source of the blue LED chip, and getting rid of the traditional packaging method, only need to attach a chip above the chip A light conversion film is enough, and the luminous effect is very close to that of the LED produced in the packaging form. Traditional packaging mixes phosphor powder in glue, and then heats and solidifies it on the dot chip to form a phosphor coating. Due to the high specificity of fluorescent materials, The particles are relatively large and easy to precipitate, so the process from the point of mixing resin on the chip to the complete curing will easily cause the fluorescent material to sink and form light spots, resulting in uneven light output and affecting the uniformity of light emission. However, the phosphor material in the light conversion film is usually uniformly dispersed, and the light emitting device made therefrom has the advantages of good light emission consistency and good light conversion effect.

Polydimethylsiloxane (Polydimethylsiloxane, PDMS) is a kind of silicone polymer, which has the advantages of good biocompatibility, low price, simple production, good light transmission, etc. It is usually made by casting method, easy to shape, It is the most widely used silicon-based organic polymer material. As far as we know, there is no report on the combination of the system red phosphor described in this paper and PDMS to make a flexible fluorescent film.

Contents of the invention

Aiming at the above-mentioned technical problems in the prior art, the present invention provides a flexible red fluorescent film. The flexible red fluorescent film should solve the problem that the fluorescent materials in the prior art are easy to form light spots, resulting in uneven light output and affecting the light emission. Technical issues of uniformity.

The invention provides a flexible red fluorescent film, which is composed of powder and organic matter, the mass ratio of the powder and organic matter is (0.1-0.3):1, and the organic matter is polydimethylsiloxane. In the powder, calculated by mass percentage of oxides, the total content of 0%<Na ₂ O+Li ₂ O+K ₂ O<6.65%, 0<MgO<8.65%, 30%<WO ₃ + The total content of MoO ₃ is <49.75%, the total content of 5%<Gd ₂ O ₃ +La ₂ O ₃ +Y ₂ O ₃ is <34.95%, and 0%<Eu ₂ O ₃ <22.28%.

The present invention also provides a method for preparing a flexible red fluorescent film, comprising the following steps:

1) Weigh each raw material according to mass percentage, the mass percentage of each raw material is: 0%<Na ₂ O+Li ₂ O+K ₂ O total content<6.65%, 0<MgO<8.65%, 30%<WO ₃ The total content of +MoO ₃ <49.75%, the total content of 5%<Gd ₂ O ₃ +La ₂ O ₃ +Y ₂ O ₃ <34.95%, 0%<Eu ₂ O ₃ <22.28%;

2) Put the phosphor raw material in an agate mortar and grind it evenly, then heat it in a muffle furnace at 1000-1200°C for 10-25 hours, cool to room temperature, and finally obtain the required red phosphor;

3) Weigh polydimethylsiloxane and curing agent, the mass ratio of dimethylsiloxane and curing agent is 10:1, mix thoroughly,

4) Weigh the phosphor powder and the solution of step 3), the mass ratio of the powder and polydimethylsiloxane is (0.1-0.3):1, mix well and pour into a container for ultrasonication;

5) Pour the above mixed solution into another container, transfer it to an oven, dry it at a temperature lower than 100° C., cool it to room temperature, and remove the solidified film to obtain a flexible red fluorescent film.

Compared with the traditional glue dispensing and coating process, the present invention independently manufactures the phosphor powder film layer, the phosphor powder is evenly distributed, the thickness of the phosphor powder film layer can be controlled, and the consistency of light and color is greatly improved. The phosphor film layer can be cut into various sizes and shapes, which is suitable for the integrated packaging of single or multi-chips. At the same time, the surface of the film layer can contain various microstructures such as microlens arrays, which can improve the uniformity and efficiency of light output. The phosphor film layer is manufactured by the method, the process is simple, the repeatability is strong, and it is suitable for large-scale and batch industrialized production. The flexible red phosphor film made of this remote red phosphor can be used in high-power LED lamps, avoiding direct contact between the phosphor material and the energy source of the blue LED chip, and improving the overall efficiency of the LED lamp.

Compared with the prior art, the technical progress of the present invention is remarkable. Combining phosphor powder and PDMS to form a film is easy to operate and low in cost, and can improve the consistency of phosphor powder coating and heat dissipation, and is suitable for large-scale and batch industrial production.

Description of drawings

Figure 1 is the excitation (λ _em = 616nm) and emission (λ _ex = 465nm) spectra of the flexible red fluorescent film.

detailed description

Example 1

1) According to the component ratio of Na ₂ O: La ₂ O ₃ : MgO: WO ₃ : Eu ₂ O ₃ =6.58: 20.74: 8.55: 49.2: 14.93 (based on oxide content), accurately weigh the total mass to be 10g NaCO ₃ , La ₂ O ₃ , 4MgCO ₃ ·Mg(OH) ₂ ·5H ₂ O, WO ₃ , Eu ₂ O ₃ were thoroughly ground in an agate mortar and then heated in a muffle furnace at 1050°C for 18 hour, cooled to room temperature, and finally obtained red phosphor.

2) Accurately weigh 0.3148g of red fluorescent powder and 2.99g of organic matter according to the mass ratio of powder to organic matter of 0.18:1; among them, accurately weigh 2.7182 g of polydimethylsiloxane (A ) and 0.2718 g curing agent (B);

3) Put the above mixture into a 10mL sample bottle, and sonicate for 40min in an ultrasonic generator;

4) Transfer the sonicated sample to a watch glass;

5) Dry at 100°C for 45 minutes to obtain a flexible red fluorescent film.

5) Using a fluorescence spectrometer of the model F-7000, test the spectral properties of the fluorescent film of this system, as shown in Figure 1, the results show that the strongest excitation peak of the phosphor powder of this system is located at 465nm, under the excitation of light of this excitation wavelength , the fluorescent film of this system exhibits red light emission with the strongest emission wavelength at 616nm, indicating that the fluorescent film of this system is a red fluorescent film that can match blue light chips.

Claims (2)

1. a kind of flexible red fluorescence film, it is characterised in that：It is made up of powder and organic matter, described powder and organic matter Mass ratio is (0.1~0.3): 1, described organic matter is dimethyl silicone polymer, in described powder, with the matter of oxide Measure percentage to calculate, 0%<Na₂O+Li₂O+K₂O total content<6.65%, 0<MgO<8.65%, 30%<WO₃+MoO₃Total content< 49.75%, 5%<Gd₂O₃+La₂O₃+Y₂O₃Total content<34.95%, 0%<Eu₂O₃<22.28%。

2. the preparation method of a kind of flexible red fluorescence film described in claim 1, it is characterised in that comprise the following steps：

1）Each raw material is weighed according to mass percent, the mass percent of each raw material is：0%<Na₂O+Li₂O+K₂O total content< 6.65%, 0<MgO<8.65%, 30%<WO₃+MoO₃Total content<49.75%, 5%<Gd₂O₃+La₂O₃+Y₂O₃Total content< 34.95%, 0%<Eu₂O₃<22.28%；

2）Phosphor raw material is placed in agate mortar and is fully ground uniformly, 1000 ~ 1200 DEG C of heating in Muffle furnace are subsequently placed in 10 ~ 25 hours, room temperature is cooled to, required red fluorescence powder is finally given；

3）Weigh dimethyl silicone polymer and curing agent, the mass ratio of dimethyl siloxane and curing agent is 10：1, it is sufficiently mixed,

4）Weigh fluorescent material and step 3）Solution, described powder and the mass ratio of dimethyl silicone polymer are (0.1~0.3) : 1, poured into after being sufficiently mixed ultrasonic in a container；

5）Above-mentioned mixed liquor is poured into another container, and is transferred in baking oven, is dried at a temperature of less than 100 DEG C Afterwards, room temperature is cooled to, the film after solidification is removed, obtains flexible red fluorescence film.