A fluorescent material, its preparation method, and its application in the preparation of thin film materials.

Abstract

The application relates to the technical field of fluorescent material preparation, and particularly discloses a fluorescent material, a preparation method thereof and application of the fluorescent material in preparing a thin film material. The preparation method of the fluorescent material comprises the following steps: (1) adding fluorescent powder into ethanol, then adding a coupling agent, stirring for 30-60 minutes to obtain fluorescent powder slurry; (2) adding an additive into the fluorescent powder slurry, continuing to stir for 30-60 minutes to obtain modified slurry; (3) putting the modified slurry into a ball mill for ball milling, obtaining ball-milled slurry after the ball milling is completed, and drying the ball-milled slurry to obtain the fluorescent material. Research shows that, compared with application of red fluorescent powder prepared by an existing method in a thin film material, the fluorescent material prepared by the method can significantly improve the tensile strength of the thin film material.

Description

Technical Field

[0001] This invention relates to the field of fluorescent material preparation technology, specifically to a fluorescent material, its preparation method, and its application in the preparation of thin film materials. Background Technology

[0002] A fluorescent film is a thin film made of fluorescent thin film material. Its main characteristic is that it can emit fluorescence under light of a specific wavelength. It is mainly used in the fields of optoelectronics, lighting, and biomedicine. Chinese invention patent 201210268609.8 discloses a red phosphor. The preparation method of the red phosphor is as follows: the carbonate of A, the carbonate of B, the oxide of C, and the oxide of D are mixed, ground, and mixed evenly; then the mixed raw materials are calcined at 1000℃-1400℃ for 6-20h, then cooled to room temperature, ground, and then calcined at 1000℃-1400℃ for 6-20h; finally, the product obtained in step (3) is cooled and crushed to obtain the phosphor. The phosphor prepared by this invention has good chemical stability and high excitation efficiency.

[0003] However, the invention found in the research that when the red phosphor prepared according to the method in Chinese invention patent 201210268609.8 is applied to thin film materials, it will reduce the tensile strength of the thin film materials, resulting in low tensile strength of the prepared thin film materials, which needs to be further improved. Summary of the Invention

[0004] In order to overcome at least one of the technical problems existing in the prior art, the present invention first provides a method for preparing fluorescent materials.

[0005] The technical solution of the present invention to solve the above-mentioned technical problems is as follows:

[0006] This invention first provides a method for preparing a fluorescent material, which includes the following steps:

[0007] (1) Add the phosphor to ethanol, then add the coupling agent, and stir for 30-60 minutes to obtain the phosphor slurry;

[0008] (2) Add additives to phosphor slurry and continue stirring for 30-60 minutes to obtain modified slurry;

[0009] (3) The modified slurry is placed in a ball mill and ball milled. After ball milling, a ball milled slurry is obtained. The ball milled slurry is dried to obtain the fluorescent material.

[0010] This invention provides a novel method for preparing fluorescent materials. Studies have shown that applying the fluorescent material prepared by the method of this invention to thin film materials can significantly improve the tensile strength of the thin film materials compared to directly applying the red phosphor prepared by the method described in Chinese Invention Patent 201210268609.8 to the thin film materials.

[0011] Preferably, the phosphor in step (1) is prepared by the following method:

[0012] Calcium carbonate, potassium carbonate, europium trioxide, and tungsten trioxide are mixed and ground. After grinding, the mixture is calcined. The calcined product is then taken to obtain the phosphor.

[0013] More preferably, the weight parts of calcium carbonate, potassium carbonate, europium trioxide, and tungsten trioxide are as follows:

[0014] Calcium carbonate 15-25 parts; potassium carbonate 2-5 parts; europium trioxide 6-10 parts; tungsten trioxide 20-30 parts.

[0015] Most preferably, the weight parts of calcium carbonate, potassium carbonate, europium trioxide, and tungsten trioxide are as follows:

[0016] Calcium carbonate 20 parts; potassium carbonate 3 parts; europium trioxide 8 parts; tungsten trioxide 25 parts.

[0017] Preferably, the calcination refers to calcining at 1100℃ for 6 hours, cooling, and then calcining at 1200℃ for 18 hours. After cooling, the powder is ground to obtain the fluorescent powder.

[0018] Preferably, the ratio of phosphor to ethanol in step (1) is 1 kg: 3-5 L.

[0019] Most preferably, the ratio of phosphor to ethanol in step (1) is 1 kg: 4 L.

[0020] Preferably, the ratio of coupling agent to ethanol in step (1) is 30-60g:3-5L.

[0021] Most preferably, the ratio of the coupling agent to ethanol in step (1) is 50g:4L.

[0022] Preferably, the ethanol refers to ethanol with a volume fraction of 80-95%.

[0023] Preferably, in step (2), the ratio of fluorescent powder slurry to additives is 3-5L:70-100g.

[0024] Most preferably, in step (2), the ratio of fluorescent powder slurry to additives is 4L:80g.

[0025] Preferably, the additive is hexadecyl lactate or oleic acid diethanolamide.

[0026] Most preferably, the additive is composed of hexadecyl lactate and oleic acid diethanolamide.

[0027] More preferably, the weight ratio of hexadecyl lactate to oleic acid diethanolamide in the additive is 2-4:1-3.

[0028] Most preferably, the weight ratio of hexadecyl lactate and oleic acid diethanolamide in the additive is 3:2.

[0029] The inventors discovered in their research that the selection of additives in step (2) of this invention is crucial. The research found that the fluorescent material prepared by using additives composed of hexadecyl lactate and oleic acid diethanolamide in step (2) can significantly improve the tensile strength of the film material. The improvement in the tensile strength of the film material is significantly higher than that of the fluorescent material prepared by using only hexadecyl lactate or oleic acid diethanolamide as additives. The use of additives composed of hexadecyl lactate and oleic acid diethanolamide to prepare the fluorescent material can synergistically improve the tensile strength of the film material.

[0030] Preferably, the media filling rate in the ball mill is 40-60%.

[0031] Preferably, the media used in the ball mill are steel balls with a diameter of 40 to 80 mm.

[0032] Preferably, the rotational speed in the ball mill is 30–50 r / min.

[0033] Preferably, the ball milling time is 1 to 2 hours.

[0034] The present invention also provides a fluorescent material prepared by the above preparation method.

[0035] The present invention also provides an application of the above-mentioned fluorescent material in the preparation of thin film materials.

[0036] Preferably, the film material refers to a film material prepared from polyethylene, polycaprolactone, and fluorescent materials.

[0037] Beneficial effects: This invention provides a novel method for preparing fluorescent materials; studies have shown that applying the fluorescent material prepared by the method of this invention to thin film materials can significantly improve the tensile strength of the thin film materials compared to directly applying the red phosphor prepared by the method described in Chinese Invention Patent 201210268609.8 to thin film materials. Detailed Implementation

[0038] The present invention will be further explained below with reference to specific embodiments, but the embodiments do not limit the present invention in any way.

[0039] Example 1: Preparation of Fluorescent Materials

[0040] (1) Add phosphor to 95% ethanol by volume, then add coupling agent (silane coupling agent KH-550), stir for 40 min to obtain phosphor slurry; wherein, the ratio of phosphor to ethanol is 1kg:4L; the ratio of coupling agent to ethanol is 50g:4L.

[0041] (2) Add an additive to the phosphor slurry and continue stirring for 40 minutes to obtain a modified slurry; wherein, the ratio of phosphor slurry to additive is 4L:80g; the additive is hexadecyl lactate.

[0042] (3) The modified slurry is placed in a ball mill and ball milled for 1.5 hours. After the ball milling is completed, the ball milled slurry is obtained. The ball milled slurry is dried to obtain the fluorescent material. The media filling rate in the ball mill is 50%, and the ball milling media is steel balls with a diameter of 60 mm and a rotation speed of 40 r / min.

[0043] The phosphor in step (1) is prepared by the following method: 20 parts of calcium carbonate, 3 parts of potassium carbonate, 8 parts of europium trioxide and 25 parts of tungsten trioxide are mixed and then 100 parts of 95% ethanol are added for grinding. After grinding, the mixture is calcined at 1100℃ for 6 hours, cooled to room temperature and then calcined at 1200℃ for 18 hours. After cooling, it is crushed to obtain the phosphor.

[0044] Example 2 Preparation of fluorescent materials

[0045] (1) Add phosphor to 95% ethanol by volume, then add coupling agent (silane coupling agent KH-550), stir for 40 min to obtain phosphor slurry; wherein, the ratio of phosphor to ethanol is 1kg:4L; the ratio of coupling agent to ethanol is 50g:4L.

[0046] (2) Add an additive to the phosphor slurry and continue stirring for 40 minutes to obtain a modified slurry; wherein, the ratio of phosphor slurry to additive is 4L:80g; the additive is oleic acid diethanolamide;

[0047] (3) The modified slurry is placed in a ball mill and ball milled for 1.5 hours. After the ball milling is completed, the ball milled slurry is obtained. The ball milled slurry is dried to obtain the fluorescent material. The media filling rate in the ball mill is 50%, and the ball milling media is steel balls with a diameter of 60 mm and a rotation speed of 40 r / min.

[0048] The preparation method of the phosphor described in step (1) is the same as in Example 1.

[0049] Example 3: Preparation of Fluorescent Materials

[0050] (1) Add phosphor to 95% ethanol by volume, then add coupling agent (silane coupling agent KH-550), stir for 40 min to obtain phosphor slurry; wherein, the ratio of phosphor to ethanol is 1kg:4L; the ratio of coupling agent to ethanol is 50g:4L.

[0051] (2) Add an additive to the phosphor slurry and continue stirring for 40 minutes to obtain a modified slurry; wherein the ratio of phosphor slurry to additive is 4L:80g; the additive is composed of hexadecyl lactate and oleic acid diethanolamide in a weight ratio of 3:2.

[0052] (3) The modified slurry is placed in a ball mill and ball milled for 1.5 hours. After the ball milling is completed, the ball milled slurry is obtained. The ball milled slurry is dried to obtain the fluorescent material. The media filling rate in the ball mill is 50%, and the ball milling media is steel balls with a diameter of 60 mm and a rotation speed of 40 r / min.

[0053] The preparation method of the phosphor described in step (1) is the same as in Example 1.

[0054] Comparative Example 1: Preparation of Fluorescent Materials

[0055] Take 20 parts of calcium carbonate, 3 parts of potassium carbonate, 8 parts of europium trioxide, and 25 parts of tungsten trioxide, mix them, and add 100 parts of 95% ethanol by volume for grinding. After grinding, calcine the mixture at 1100℃ for 6 hours, cool it to room temperature, and then calcine it at 1200℃ for 18 hours. After cooling, grind it to obtain the fluorescent material.

[0056] Experimental Example 1

[0057] Ten parts by weight of the fluorescent materials prepared in Examples 1-3 and Comparative Example 1 were mixed with 60 parts by weight of polyethylene and 40 parts by weight of polycaprolactone, and then melt-extruded through a twin-screw extruder to obtain the film materials. The tensile strength of each film material was tested according to the method in GB / T 1040.1-2018. The test results are shown in Table 1.

[0058] The polyethylene used in this experimental example is low-density polyethylene of Yanshan Petrochemical with the grade 1C7A; the polycaprolactone used is low-density polyethylene of Solvay, USA with the grade 6800.

[0059] Table 1. Effect of the fluorescent material of the present invention on the tensile strength of the prepared thin film material

[0060] Tensile strength of thin film materials Fluorescent material prepared in Example 1 12.7MPa Fluorescent materials prepared in Example 2 13.5MPa Fluorescent material prepared in Example 3 16.6MPa Fluorescent materials prepared in Comparative Example 1 9.6MPa

[0061] As can be seen from the experimental data in Table 1, the tensile strength of the thin film material prepared using the fluorescent materials described in Examples 1 and 2 is significantly higher than that of the thin film material prepared using the fluorescent material described in Comparative Example 1. This indicates that applying the fluorescent material prepared by the method of the present invention to the thin film material can significantly improve the tensile strength of the thin film material compared to applying the red phosphor prepared according to the method described in Chinese Invention Patent 201210268609.8.

[0062] As can be seen from the experimental data in Table 1, the tensile strength of the film material prepared using the fluorescent material described in Example 3 is significantly higher than that of the film material prepared using the fluorescent material described in Comparative Example 1; it is also significantly higher than that of the film material prepared using the fluorescent materials described in Examples 1 and 2. This indicates that the selection of the auxiliary agent in step (2) of the present invention is crucial. The study found that the fluorescent material prepared by simultaneously using an auxiliary agent composed of hexadecyl lactate and oleic acid diethanolamide in step (2) can significantly improve the tensile strength of the film material; its improvement on the tensile strength of the film material is significantly higher than that of the fluorescent material prepared by using only hexadecyl lactate or oleic acid diethanolamide as an auxiliary agent; the use of an auxiliary agent composed of hexadecyl lactate and oleic acid diethanolamide to prepare the fluorescent material can synergistically improve the tensile strength of the film material.

Claims

1. A method for producing a fluorescent material, characterized by, The preparation method comprises the following steps: (1) adding the fluorescent powder into ethanol, then adding coupling agent, stirring for 30-60 minutes to obtain fluorescent powder slurry; (2) adding auxiliary agent into the fluorescent powder slurry, continuing to stir for 30-60 minutes to obtain modified slurry; (3) putting the modified slurry into a ball mill to ball mill, drying the ball milled slurry to obtain the fluorescent material; the coupling agent is silane coupling agent KH-550; the auxiliary agent is composed of hexadecyl lactate and oleic acid diethanol amide.

2. The method of claim 1, wherein the method is performed in the presence of a reducing agent. The fluorescent powder in step (1) is prepared by the following method: mixing calcium carbonate, potassium carbonate, europium trioxide and tungsten trioxide, grinding, calcining the ground mixture, and obtaining the fluorescent powder after calcination.

3. The method of claim 1, wherein the method is performed in the presence of a reducing agent. The weight parts of calcium carbonate, potassium carbonate, europium trioxide and tungsten trioxide are as follows: calcium carbonate 15-25 parts; potassium carbonate 2-5 parts; europium trioxide 6-10 parts; tungsten trioxide 20-30 parts.

4. The method of claim 1, wherein the method is performed in the presence of a reducing agent. The use amount ratio of the fluorescent powder in step (1) to ethanol is 1 kg:3-5 L.

5. The method for preparing fluorescent materials according to claim 1, characterized in that, The use amount ratio of the coupling agent in step (1) to ethanol is 30-60 g:3-5 L.

6. The method of claim 1, wherein the phosphor is prepared by a process comprising: The ethanol refers to ethanol with a volume fraction of 80-95%.

7. The method for preparing fluorescent materials according to claim 1, characterized in that, The use amount ratio of the fluorescent powder slurry in step (2) to auxiliary agent is 3-5 L:70-100 g.

8. The method for preparing fluorescent materials according to claim 1, characterized in that, The auxiliary agent is hexadecyl lactate or oleic acid diethanol amide.

9. The fluorescent material prepared by the preparation method in any one of claims 1-8.

10. The application of the fluorescent material in claim 9 in preparing thin film material.