METHOD FOR PREPARING MANGANESE-DOPED RED PHOSPHOR, PRODUCT, DEVICE, AND BACKLIGHT MODULE

Abstract

Disclosed are a preparation method for manganese-doped red phosphor, a device and a backlight module including the product. The method includes: 1) mixing A.sub.2BF.sub.6 polycrystalline particles with mill balls; 2) mixing A.sub.2BF.sub.6 powder obtained after ball-milling with a hydrofluoric acid for secondary crystallization; 3) filtering out solid particles in A.sub.2BF.sub.6 and hydrofluoric acid solution after the secondary crystallization; 4) performing ion exchange between A.sub.2BF.sub.6 particles and A.sub.2BF.sub.6; and 5) filtering out solid particles to obtain a filter cake, and performing drying treatment to obtain manganese-doped red phosphor.

Claims

1. A preparation method for manganese-doped red phosphor, wherein the method comprises: 1) mixing A.sub.2BF.sub.6 polycrystalline particles with grinding balls, wherein a mass ratio of the A.sub.2BF.sub.6 polycrystalline particles to the grinding balls is 1:1 to 1:2.5, and then ball-milling for 30 minutes to 120 minutes, wherein A is a monovalent cation, comprising one or a combination of a group consist of a potassium ion, a hydrogen ion, a lithium ion, a sodium ion and a cesium ion, and B is a tetravalent cation, comprising one or a combination of a group consist of a titanium ion a silicon ion, a germanium ion, a tin ion, and a zirconium ion; 2) mixing A.sub.2BF.sub.6 powder obtained after ball-milling with a hydrofluoric acid, a mass fraction of the hydrofluoric acid is 30% to 59%, wherein a mass ratio of the A.sub.2BF.sub.6 powder obtained after ball-milling to the hydrofluoric acid is 1:1 to 2.5:1, and then at a revolving speed of 1 RPM to 1200 RPMs, stirring for 12 hours to 72 hours for secondary crystallization treatment; 3) filtering out solid particles in A.sub.2BF.sub.6 and hydrofluoric acid solution after the secondary crystallization, to obtain A.sub.2BF.sub.6 particles after the secondary crystallization; 4) according to a molar ratio of A.sub.2BF.sub.6 and A.sub.2MnF.sub.6 which is 93:7 to 90:10, weighing the A.sub.2BF.sub.6 particles after the secondary crystallization and A.sub.2MnF.sub.6, and then firstly dissolving A.sub.2MnF.sub.6 in a hydrofluoric acid, a mass fraction of the hydrofluoric acid is 30% to 59%, and then adding the A.sub.2BF.sub.6 particles after the secondary crystallization to a solution comprising the A.sub.2MnF.sub.6 and the hydrofluoric acid, and continuously stirring for 10 minutes to 360 minutes for ion exchange, wherein a ratio of a total mass of A.sub.2BF.sub.6 and A.sub.2MnF.sub.6 to a mass of the hydrofluoric acid is 1:1 to 4:1; and 5) filtering out solid particles in solution after the ion exchange, to obtain a filter cake, and then drying the filter cake to obtain the manganese-doped red phosphor.

2. The preparation method for the manganese-doped red phosphor according to claim 1, wherein the secondary crystallization treatment process in the step 2) is performed in a sealed reactor.

3. The preparation method for the manganese-doped red phosphor according to claim 1, wherein the step 3) comprises: under conditions of a vacuum degree of 60 Pa to 200 Pa and a flow rate of 60 L/min to 100 L/min, performing vacuum suction filtration treatment on the A.sub.2BF.sub.6 and hydrofluoric acid solution after the secondary crystallization, to obtain the A.sub.2BF.sub.6 particles after the secondary crystallization.

4. The preparation method for the manganese-doped red phosphor according to claim 1, wherein a preparation method for A.sub.2MnF.sub.6 in the step 4) comprises: A: dissolving potassium hydrogen fluoride in a hydrofluoric acid, a mass fraction of the hydrofluoric acid is 30% to 59%, wherein a mass ratio of the potassium hydrogen fluoride to the hydrofluoric acid is 2:10 to 4:10; and at a revolving speed of 10 RPM to 1000 RPM, stirring for 15 minutes to 40 minutes; B: adding potassium permanganate while stirring, wherein a mass ratio of the potassium permanganate to the potassium hydrogen fluoride is 1:5 to 2:5; C: using a hydrogen peroxide to titrate solution after adding the potassium permanganate to be golden yellow, a mass fraction of the hydrogen peroxide is 25% to 40%; D: putting the titrated solution together with a reactor into an ice-water mixture at 0° C. to 5° C. and standing for 15 minutes to 40 minutes, filtering out a precipitate, and then using acetone to repeatedly wash the precipitate to be neutral; and E: drying the washed precipitate for 1 hour to 4 hours under conditions of a temperature of 60° C. to 90° C. and a vacuum degree of 90 Pa to 500 Pa, to obtain A.sub.2MnF.sub.6.

5. The preparation method for the manganese-doped red phosphor according to claim 1, wherein the step 5) comprises: under conditions of a vacuum degree of 60 Pa to 200 Pa and a flow rate of 60 L/min to 100 L/min, performing vacuum suction filtration treatment on the solution after ion exchange, to obtain a filter cake, and then using acetone to repeatedly wash the filter cake to be neutral, and then drying the filter cake for 1 hour to 4 hours under conditions of a temperature of 60° C. to 90° C. and a vacuum of 90 Pa to 500 Pa, to obtain the manganese-doped red phosphor.

6. (canceled)

7. A product prepared by the preparation method for the manganese-doped red phosphor according to claim 1.

8. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 1, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

9. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 1.

10. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 2, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

11. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 3, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

12. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 4, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

13. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 5, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

14. A device packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 6, wherein the device comprises: an excitation source, phosphor, an electrode, a packaging material, and a support, wherein the electrode is connected with the excitation source; the phosphor is distributed in the packaging material, and arranged around the excitation source; and the support carries the excitation source, the electrode, and the packaging material.

15. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 2.

16. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 3.

17. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 4.

18. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 5.

19. A backlight module packaged by a product prepared by the preparation method for the manganese-doped red phosphor according to claim 6.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0040] FIG. 1 is a structure schematic diagram of a device packaged by manganese-doped red phosphor provided by an embodiment of the disclosure.

[0041] FIG. 2 is a test result of the emission intensity of products prepared in Embodiments 1 to 4 provided by an embodiment of the disclosure.

[0042] FIG. 3 is a test result of the emission intensity of products prepared in Embodiments 5 to 8 provided by an embodiment of the disclosure.

[0043] FIG. 4 is a test result of the emission intensity of products prepared in Embodiments 9 to 12 provided by an embodiment of the disclosure.

[0044] FIG. 5 is a test result of the emission intensity of products prepared in Embodiments 13 to 16 provided by an embodiment of the disclosure.

[0045] FIG. 6 is a test result of the emission intensity of products prepared in Embodiments 17 to 19 provided by an embodiment of the disclosure.

[0046] FIG. 7 is a schematic diagram of an emission spectrum of a material prepared in the embodiment of the disclosure and a contrast example provided by an embodiment of the disclosure.

DETAILED DESCRIPTION OF THE EMBODIMENTS

[0047] Embodiments of the disclosure are described in detail below. The embodiments are implemented on the premise of technical schemes of the disclosure, and detailed implementation modes and specific operation processes are provided, but a scope of protection of the disclosure is not limited to the following embodiments.

[0048] The embodiments of the disclosure provide a preparation method for manganese-doped red phosphor, a product, a device and a backlight module, and the preparation method for the manganese-doped red phosphor provided by the embodiment of the disclosure are firstly introduced below.

[0049] An embodiment of the disclosure provides a preparation method for manganese-doped red phosphor, the method includes:

[0050] 1) K.sub.2TiF.sub.6 polycrystalline particles purchased from Aladdin Reagent Network with an article number P112424 were mixed with grinding balls, and the mass ratio of the K.sub.2TiF.sub.6 polycrystalline particles to the grinding balls was 1:1. A mixture of the K.sub.2TiF.sub.6 polycrystalline particles and the grinding balls was loaded into a polytetrafluoroethylene reactor, and ball-milling was performed for 30 min in a MSK-SFM-3-type high-speed vibration ball mill produced by Hefei Kejing Material Technology Co., Ltd.

[0051] 2) In the polytetrafluoroethylene reactor, K.sub.2TiF.sub.6 powder obtained after ball-milling was mixed with a hydrofluoric acid, the mass fraction of the hydrofluoric acid was 30%, herein the mass ratio of the K.sub.2TiF.sub.6 powder obtained after ball-milling to the hydrofluoric acid was 1:1, and the hydrofluoric acid was an analytical pure hydrofluoric acid produced by Tianjin Hengxing Chemical Reagent Manufacture Co., Ltd. Then, the polytetrafluoroethylene reactor was sealed, and an HJ-4A-type digital display temperature controlled magnetic stirrer produced by Changzhou Guoyu Instrument Manufacture Co., Ltd. was used to treat the mixture of the hydrofluoric acid and the K.sub.2TiF.sub.6 powder obtained after ball-milling, at a revolving speed of 1 RPM to 1200 RPMs stirring was performed for 12 hours to 72 hours for secondary crystallization treatment.

[0052] 3) An SHZ-BD(III) polytetrafluoroethylene vacuum filter produced by Yangshen Technology Instrument (Shanghai) Co., Ltd., under conditions of a vacuum degree of 60 Pa to 200 Pa and a flow rate of 60 L/min to 100 L/min, was used to perform vacuum suction filtration treatment on K.sub.2TiF.sub.6 and hydrofluoric acid solution after the secondary crystallization, to obtain K.sub.2TiF.sub.6 particles after the secondary crystallization.

[0053] 4) Firstly, K.sub.2MnF.sub.6 was prepared according to the following method: A: In a polytetrafluoroethylene beaker, according to the mass ratio of analytical pure potassium hydrogen fluoride produced by Shanghai Sansi Zhuoyue Chemical Co., Ltd. to the hydrofluoric acid which was 2:10 to 4:10, the potassium hydrogen fluoride was dissolved in the hydrofluoric acid, the mass fraction of hydrofluoric acid was 30% to 59%, and at a revolving speed of 10 RPMs to 1000 RPMs, an HJ-4A digital display temperature controlled magnetic stirrer produced by Changzhou Guoyu Instrument Manufacture Co., Ltd. was used to stir for 30 minutes. B: While stirring, analytical pure potassium permanganate produced by Sinopharm Group Chemical Reagent Co., Ltd. (National Pharmaceutical Code 10017308) was added, herein the mass ratio of the potassium permanganate to the potassium hydrogen fluoride was 1:5 to 2:5. C: Analytical pure hydrogen peroxide produced by Sinopharm Group Chemical Reagent Co., Ltd. (National Pharmaceutical Code 10011208) with a mass fraction of 25% to 40% was used to titrate solution after adding the potassium permanganate to be golden yellow, until the color of the solution was not changed along with dropping of the hydrogen peroxide. D: The titrated solution together with a reactor was put into ice-water mixed solution at 0° C. to 5° C. and standing was performed for 15 minutes to 40 minutes, a precipitate is filtered out, and then analytical pure acetone (National Pharmaceutical Code 10000418) produced by Sinopharm Group Chemical Reagent Co., Ltd. was used to repeatedly wash the precipitate to be neutral. E: Then, a DZF-6020 vacuum dryer produced by Shanghai Boxun Industrial Co., Ltd. was used to dry the washed precipitate under conditions of a temperature of 60° C. to 90° C. and a vacuum degree of 90 Pa to 500 Pa for 1 hour to 4 hours, to obtain K.sub.2MnF.sub.6.

[0054] 5) According to the molar ratio of K.sub.2TiF.sub.6 to K.sub.2MnF.sub.6 which was 93:7 to 90:10, the K.sub.2TiF.sub.6 particles after the secondary crystallization and K.sub.2MnF.sub.6 were weighed, and then firstly K.sub.2MnF.sub.6 was dissolved in the hydrofluoric acid, the mass fraction of the hydrofluoric acid was 30% to 59% and K.sub.2TiF.sub.6 was added to solution of K.sub.2MnF.sub.6 and hydrofluoric acid, and the stirring was continuously performed for 10 minutes to 360 minutes for ion exchange, herein a ratio of the total mass of K.sub.2TiF.sub.6 and K.sub.2MnF.sub.6 to the mass of the hydrofluoric acid was 1:1 to 4:1.

[0055] 6) Under conditions of a vacuum degree 60 Pa to 200 Pa and a flow rate 60 L/min to 100 L/min, vacuum suction filtration treatment was performed on the solution after the ion exchange, to obtain a filter cake, and then the analytical pure acetone (National Pharmaceutical Code 10000418) produced by Sinopharm Group Chemical Reagent Co., Ltd. was used to repeatedly wash the filter cake to be neutral, and then the DZF-6020 vacuum dryer produced by Shanghai Boxun Industrial Co., Ltd., under conditions of a temperature of 60° C. to 90° C. and a vacuum degree of 90 Pa to 500 Pa, was used to dry the filter cake for 1 hour to 4 hours, to obtain the manganese-doped red phosphor, namely K.sub.2TiF.sub.6:Mn.sup.4+.

[0056] An embodiment of the disclosure further provides a product prepared according to the above method.

[0057] An embodiment of the disclosure further provides a device packaged by a product prepared according to the above method, and FIG. 1 is a structure schematic diagram of a device packaged by manganese-doped red phosphor provided by an embodiment of the disclosure, as shown in FIG. 1, the device 100 includes: an excitation source 101, phosphor 103, an electrode 105, a packaging material 107 and a support 109, herein,

[0058] the electrode 105 is connected with the excitation source 101; specifically, the excitation source 101 can be an LED chip;

[0059] the phosphor 103 is distributed in the packaging material 107, and arranged around the excitation source 101; specifically, the packaging material 107 can be a transparent silica gel; and

[0060] the support 109 carries the excitation source 101, the electrode 105, and the packaging material 107.

[0061] An embodiment of the disclosure further provides a backlight module packaged by a product prepared according to the above method.

[0062] Technical schemes in the embodiments of the disclosure are clearly and completely described below, herein Table 1 is a table of process parameters used in Embodiments 1 to 9 of the disclosure; and Table 2 is a table of process parameters used in Embodiments 10 to 19 of the disclosure; as shown in Table 1 and Table 2.

TABLE-US-00001 TABLE 1 Embodiment number 1 2 3 4 5 6 7 8 9 Step Ball to material 1:1 1:1 1:1 1:1 1.5:1   1.5:1   1.5:1   1.5:1   2:1 1 ratio Ball-milling time 30 60 90 120 30 60 90 120 30 length (min) Step Hydrofluoric acid 30 35 40 45 50 55 59 30 35 2 mass fraction (%) Mass ratio of 1:1   1:1.5 1:2   1:2.5   1:2.5 1:2   1:1.5 1:1   1:1.5 potassium fluorotitanate to hydrofluoric acid Stirring speed 400 600 800 1200 800 1200 400 600 12000 (RPM) Crystallization 24 36 48 60 36 24 60 48 48 time length (h) Step Suction filtration 60 70 80 90 100 110 120 130 140 3 vacuum degree (Pa) Suction filtration 60 65 70 75 80 85 90 95 100 flow rate (L/min) Step Mass ratio of  2:10 2.5:10   3:10 3.5:10   4:10  2:10 2.5:10   3:10 3.5:10  4 potassium hydrogen fluoride to hydrofluoric acid Hydrofluoric acid 30 35 40 45 50 55 59 30 35 mass fraction (%) Stirring speed 10 20 40 60 80 100 200 300 400 (RPM) Stirring time 15 17 20 22 25 27 30 15 17 length (min) Mass ratio of 1:5 1.2:5   1.5:5   1.7:5   2:5 1:5 1.2:5   1.5:5   1.7:5   potassium permanganate to potassium hydrogen fluoride Hydrogen 25 27 30 32 35 37 40 25 27 peroxide mass fraction (%) Ice-water mixture 0 1 2 3 4 5 0 1 2 temperature (° C.) Standing time 15 17 20 22 25 27 30 32 35 length (min) Drying 60 65 70 75 80 85 90 60 65 temperature (° C.)/ Drying vacuum 90 120 150 180 200 240 280 320 360 degree (Pa) Drying time length 1 1.2 1.4 1.6 1.8 2 2.2 2.4 2.6 (h) Step Molar ratio of 90:10 91:9  92:8  93:7  90:10 91:9  92:8  93:7  90:10 5 potassium fluorotitanate to potassium fluoromanganate Hydrofluoric acid 30 35 40 45 50 55 59 30 35 mass fraction (%) Stirring time 10 20 40 60 80 100 120 140 160 length (min) Ratio of total 1:1 1.5:1   2:1 2.5:1   3:1 3.5:1   4:1 1:1 1.5:1   mass of potassium fluorotitanate and potassium fluoromanganate to mass of hydrofluoric acid Step6 Suction filtration 60 70 80 90 100 110 120 130 140 vacuum degree (Pa) Suction filtration 60 65 70 75 80 85 90 95 100 flow rate (L/min) Drying 60 65 70 75 80 85 90 60 65 temperature (° C.) Drying vacuum 90 120 150 180 210 240 270 300 330 degree (Pa) Drying time length 1 1.5 2 2.5 3 3.5 4 1 1.5 (h)

TABLE-US-00002 TABLE 2 Embodiment number 10 11 12 13 14 15 16 17 18 19 Step Ball to material 2:1 2:1 2:1 2.5:1   2.5:1   2.5:1   2.5:1   2:1 2:1 2:1 1 ratio Ball-milling time 60 90 120 30 60 90 120 90 90 90 length (min) Step2 Hydrofluoric 40 45 50 55 59 30 35 40 40 40 acid mass fraction (%) Mass ratio of 1:1   1:2.5 1:2 1:2 1:2   1:1.5   1:1.5   1:1.5   1:1.5   1:1.5 potassium fluorotitanate to hydrofluoric acid Stirring speed 800 600 400 600 400 1200 800 400 400 400 (RPM) Crystallization 60 24 36 60 48 36 24 36 48 60 time length (h) Step Suction filtration 150 160 170 180 190 200 190 180 180 180 3 vacuum degree (Pa) Suction filtration 60 65 70 75 80 85 90 95 95 95 flow rate (L/min) Step4 Mass ratio of  4:10  2:10 2.5:10   3:10 3.5:10   4:10  2:10 2.5:10  2.5:10  2.5:10  potassium permanganate to potassium hydrogen fluoride Hydrofluoric 40 45 50 55 59 30 35 40 40 40 acid mass fraction (%) Stirring speed 500 600 700 800 900 1000 900 800 800 800 (RPM) Stirring time 20 22 25 27 30 15 17 20 30 30 length (min) Mass ratio of 2:5 1:5 1.2:5   1.5:5   1.7:5    2:5 1:5 1.2:5   1.2:5   1.2:5   potassium permanganate to potassium hydrogen fluoride Hydrogen 30 32 35 37 40 25 27 30 30 30 peroxide mass fraction (%) Ice-water 3 4 5 0 1 2 3 4 4 4 mixture temperature (° C.) Standing time 37 40 15 17 20 22 25 27 length (min) Drying 70 75 80 85 90 60 65 70 70 70 temperature (° C.) Drying vacuum 400 420 440 480 500 90 120 150 150 150 degree (Pa) Drying time 2.8 3 3.2 3.4 3.6 3.8 4 1 3 3 length (h) Step Molar ratio of 91:9  92:8  93:7  90:10 91:9  92:8  93:7  90:10 92:8  92:8  5 potassium fluorotitanate to potassium fluoromanganate Hydrofluoric 40 45 50 55 59 30 35 40 40 40 acid mass fraction (%) Stirring speed 500 600 700 800 900 1000 900 800 400 400 (RPM) Stirring time 180 200 220 240 260 280 300 320 340 360 length (min) Ratio of total 2:1 2.5:1   3:1 3.5:1   4:1 1:1 1.5:1   2:1 4:1 4:1 mass of potassium fluorotitanate and potassium fluoromanganate to mass of hydrofluoric acid Step Suction filtration 150 160 170 180 190 200 190 180 180 180 6 vacuum degree (Pa) Suction filtration 60 65 70 75 80 85 90 95 95 95 flow rate (L/min) Drying 70 75 80 85 90 60 65 70 70 70 temperature (° C.) Drying vacuum 360 390 420 450 480 500 470 440 440 440 degree (Pa) Drying time 2 2.5 3 3.5 4 1 1.5 4 4 4 length (h)

[0063] Relative Light Intensity Test

[0064] An F4600 fluorescence spectrometer produced by Hitachi Manufacture Co., Ltd. is used to test the products prepared in Embodiments 1 to 19, and test results are shown in Table 3.

[0065] Table 3 is the test results of luminous intensities, color coordinates, color temperatures and color rendering indexes of the products prepared in Embodiments 1 to 19 provided by the embodiments of the disclosure, herein the relative intensity is obtained by integrating an emission spectrum within a range of 580 nm to 680 nm; and the color coordinates, correlated color temperatures, and color rendering indexes are calculated by using “CIE13_3w.exe” software.

TABLE-US-00003 TABLE 3 Correlated color Color Relative Color temperature rendering intensity coordinate (x, y) (K) index Ra Embodiment 1 55.94242 (0.6877, 0.3121) 1000 12.03 Embodiment 2 89.87714 (0.6882, 0.3117) 1000 11.63 Embodiment 3 84.27215 (0.6880, 0.3119) 1000 11.36 Embodiment 4 50.64414 (0.6879, 0.3120) 1000 11.24 Embodiment 5 80.00677 (0.6882, 0.3116) 1000 11.64 Embodiment 6 67.25242 (0.6880, 0.3119) 1000 11.67 Embodiment 7 94.9639 (0.6884, 0.3114) 1000 11.13 Embodiment 8 57.37577 (0.6881, 0.3118) 1000 10.47 Embodiment 9 82.79778 (0.6883, 0.3115) 1000 11.36 Embodiment 100 (0.6883, 0.3116) 1000 11.15 10 Embodiment 92.70986 (0.6884, 0.3115) 1000 11.12 11 Embodiment 83.39078 (0.6883, 0.3116) 1000 10.95 12 Embodiment 74.87309 (0.6884, 0.3115) 1000 11.34 13 Embodiment 81.62602 (0.6884, 0.3115) 1000 11.19 14 Embodiment 85.48093 (0.6883, 0.3116) 1000 11.17 15 Embodiment 62.66306 (0.6886, 0.3113) 1000 11.10 16 Embodiment 82.61542 (0.6880, 0.3245) 1000 11.15 17 Embodiment 84.40983 (0.6882, 0.3546) 1000 11.19 18 Embodiment 73.06636 (0.6884, 0.1323) 1000 11.14 19

[0066] FIG. 2 is a test result of the emission intensity of products prepared in Embodiments 1 to 4 provided by an embodiment of the disclosure; FIG. 3 is a test result of the emission intensity of products prepared in Embodiments 5 to 8 provided by an embodiment of the disclosure; FIG. 4 is a test result of the emission intensity of products prepared in Embodiments 9 to 12 provided by an embodiment of the disclosure; FIG. 5 is a test result of the emission intensity of products prepared in Embodiments 13 to 16 provided by an embodiment of the disclosure; and FIG. 6 is a test result of the emission intensity of products prepared in Embodiments 17 to 19 provided by an embodiment of the disclosure.

[0067] In FIGS. 2 to 5, 1 represents the test result of the product prepared in Embodiment 1, and so on. It can be seen from FIGS. 2 to 5 that the luminous intensity of the products prepared in the embodiment of the disclosure is between 900 to 1300.

[0068] A F4600 fluorescence spectrometer produced by Hitachi Manufacture Co., Ltd. is used to perform a relative luminous intensity test according to the above dosage, and FIG. 7 is a schematic diagram of an emission spectrum of a material prepared in the embodiment of the disclosure and a contrast example provided by an embodiment of the disclosure, as shown in FIG. 7, K.sub.2TiF.sub.6:Mn.sup.4+ is an average value of the relative strength of the products prepared by using Embodiments 1 to 19 of the disclosure, and K.sub.2SiF.sub.6:Mn.sup.4+ is KSF red powder (brand name BR-3011C) produced by Mitsubishi Chemical Corporation; K.sub.2GeF.sub.6:Mn.sup.4+ is KGF red powder (brand name 690F-103B) produced by Advanced Material Research Co., Ltd. It is apparent that, through applying the embodiments of the disclosure, the dosage of phosphor can be reduced.

[0069] External Quantum Efficiency Comparison Test

[0070] A QY-2000-type integrating sphere fluorescence spectrometer produced by Tianjin Dongfang Kejie Technology Co., Ltd. is used to test the products prepared in Embodiments 1 to 19, the KSF (K.sub.2SiF.sub.6:Mn.sup.4+) red powder (brand name BR-301/C) produced by Mitsubishi Chemical Corporation, and the KGF (K.sub.2GeF.sub.6:Mn.sup.4+) red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd. Test results are as shown in Table 4.

[0071] Table 4 is a result comparison table of testing the products prepared in Embodiments 1 to 19, the KSF (K.sub.2SiF.sub.6:Mn.sup.4+) red powder (brand name BR-301/C) produced by Mitsubishi Chemical Corporation, and the KGF (K.sub.2GeF.sub.6:Mn.sup.4+) red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd. according to the embodiments of the disclosure.

TABLE-US-00004 TABLE 4 External Absolute Light quantum quantum absorption Sample yield (%) yield (%) efficiency (%) Embodiment 1 69.61% 91.08% 74.24% Embodiment 2 69.35% 92.75% 74.69% Embodiment 3 69.09% 93.06% 74.24% Embodiment 4 69.41% 91.56% 76.58% Embodiment 5 69.51% 91.57% 77.34% Embodiment 6 69.47% 91.84% 77.34% Embodiment 7 69.46% 92.04% 76.53% Embodiment 8 69.34% 92.67% 76.84% Embodiment 9 69.54% 91.42% 76.28% Embodiment 10 69.10% 93.06% 78.68% Embodiment 11 69.34% 91.43% 78.24% Embodiment 12 69.72% 92.45% 76.58% Embodiment 13 69.91% 93.54% 77.34% Embodiment 14 69.27% 92.46% 78.54% Embodiment 15 69.35% 91.57% 76.35% Embodiment 16 69.25% 93.47% 76.82% Embodiment 17 69.34% 93.54% 76.24% Embodiment 18 69.35% 92.45% 78.24% Embodiment 19 69.47% 92.04% 75.28% Grinm 66.87%   100% 66.87% Advanced Materials Co., Ltd. Mitsubishi 56.10% 85.57% 65.56% Chemical Corporation

[0072] It can be seen from Table 4 that the external quantum efficiency, absolute quantum efficiency and absorption rate of the products prepared in Embodiments 1 to 19 of the disclosure are all higher than the KSF red powder (brand name BR-301/C) produced by Mitsubishi Chemical Corporation and the KGF (K.sub.2GeF.sub.6:Me) red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd.

[0073] Phosphor Dosage Comparison Test

[0074] The products prepared in Embodiments 1 to 19, the KSF red powder (brand name BR-3011C) produced by Mitsubishi Chemical Corporation, and the KGF red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd. are used to be packaged into a white light LED device of a display backlight source, and a weight test is performed. Test results are as shown in Table 5.

[0075] Table 5 is a result comparison table of testing the products prepared in Embodiments 1 to 19, the KSF red powder (brand name BR-301/C) produced by Mitsubishi Chemical Corporation, and the KGF red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd. according to the embodiments of the disclosure.

TABLE-US-00005 TABLE 5 Dosage Theron green Packaging Number (g) powder (g) glue (g) Embodiment 1 0.732 0.2874 2.5 Embodiment 2 0.732 0.2874 2.5 Embodiment 3 0.732 0.2874 2.5 Embodiment 4 0.732 0.2874 2.5 Embodiment 5 0.732 0.2874 2.5 Embodiment 6 0.732 0.2874 2.5 Embodiment 7 0.732 0.2874 2.5 Embodiment 8 0.732 0.2874 2.5 Embodiment 9 0.732 0.2874 2.5 Embodiment 10 0.732 0.2874 2.5 Embodiment 11 0.732 0.2874 2.5 Embodiment 12 0.732 0.2874 2.5 Embodiment 13 0.732 0.2874 2.5 Embodiment 14 0.732 0.2874 2.5 Embodiment 15 0.732 0.2874 2.5 Embodiment 16 0.732 0.2874 2.5 Embodiment 17 0.732 0.2874 2.5 Embodiment 18 0.732 0.2874 2.5 Embodiment 19 0.732 0.2874 2.5 Grinm Advanced 0.972 0.2874 2.5 Materials Co., Ltd. Mitsubishi 0.972 0.2874 2.5 Chemical Corporation

[0076] It can be seen from Table 5 that the amounts of the products prepared in Embodiments 1 to 19 of the disclosure are all less than that of the KSF red powder (brand name BR-301/C) produced by Mitsubishi Chemical Corporation, and the KGF red powder (brand name 690F-103B) produced by Grinm Advanced Materials Co., Ltd.

[0077] The above are only the preferred embodiments of the disclosure, and are not intended to limit the disclosure. Any modifications, equivalent replacements and improvements and the like made within the spirit and principle of the disclosure shall be included in a scope of protection of the disclosure.