Yellow fluorescent glass as well as preparation method and application thereof

Through the specific composition of glass powder and yellow phosphor ratio and low-temperature stirring sintering process, the problem of the degradation of luminous performance of yellow fluorescent glass during high-temperature sintering is solved, and the application of high-efficiency white LED is realized.

CN120504494APending Publication Date: 2025-08-19BAOTOU RESEARCH INSTITUTE OF RARE EARTHS

Patent Information

Application Number
CN202510643144.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-19
Publication Date
2025-08-19

AI Technical Summary

Technical Problem

The existing yellow fluorescent glass can easily lead to a decrease in the luminescence performance of the phosphor during high-temperature sintering, and the interface reaction is serious, affecting the luminescence efficiency.

Method used

The ratio of specific composition glass powder and yellow phosphor is adopted, and the yellow fluorescent glass is prepared through low-temperature stirring and low-temperature sintering processes, including ball milling, drying, sifting powder, low-temperature stirring and other steps to ensure that the phosphor remains active in the glass liquid.

Benefits of technology

It improves the luminous efficiency of yellow fluorescent glass under blue light excitation, and has a moderate color temperature, which extends the lamp life and reduces energy consumption.

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Abstract

The invention discloses yellow fluorescent glass as well as a preparation method and application thereof. The yellow fluorescent glass comprises the following raw materials: glass powder and yellow fluorescent powder, wherein the weight of the yellow fluorescent powder is 22-60wt% of the weight of the glass powder; the glass powder is prepared from the following components in percentage by mole: 5 to 15 mol percent of SiO2, 20 to 30 mol percent of P2O5, 35 to 45 mol percent of Al2O3, 15 to 25 mol percent of Na2O and 1 to 10 mol percent of K2O. The luminous efficiency of white light generated by the yellow fluorescent glass under the excitation of blue light is at least 1471m / W.
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Description

Technical Field

[0001] The invention relates to yellow fluorescent glass and a preparation method and application thereof. Background Art

[0002] White light LEDs converted from fluorescent materials are widely used in a variety of fields, including indoor lighting, display screens, and automotive lighting, due to their long lifespan, low energy consumption, and environmental friendliness. They are gradually replacing halogen and incandescent lamps and becoming the next generation of lighting tools. As application scenarios continue to expand, those skilled in the art are constantly developing new phosphor conversion materials for white light LEDs to address the poor thermal stability, yellowing, and aging issues of traditional organic packaging materials. Using glass with good thermal stability as a substrate, the yellow phosphor YAG:Ce(Y3Al5O 12 :Ce 3+ Yellow fluorescent glass, formed by a molten-glass substrate (e.g., a molten-glass substrate) with a molten-glass substrate, has attracted extensive attention and research due to its low production cost, simple process, and excellent performance. However, composite materials composed of glass components and phosphor powders often require high-temperature sintering. Prolonged exposure to high temperatures can lead to significant phosphor loss, and an interface layer can form between the phosphor powder and the glass powder, reducing the phosphor's luminescence performance. To address this issue, those skilled in the art have sought to improve yellow fluorescent glass and its production process by addressing factors such as the sintering temperature and the composite structure between the substrate component and the phosphor powder.

[0003] CN103396007A discloses a fluorescent glass sheet for white light LEDs. The fluorescent glass sheet comprises a transparent glass substrate layer and a fluorescent glass layer fused to the surface. The fluorescent glass layer is formed by coating a base flux glass powder with a certain proportion of fluorescent powder on the glass substrate and firing at 550-850°C. The glass powder used contains a high content of B2O3, and the glass powder and fluorescent powder must be co-sintered to form the fluorescent glass, which can easily reduce the luminescence performance of the fluorescent powder. The fluorescent glass sheet also requires a glass substrate, resulting in poor transmittance of the fluorescent glass.

[0004] CN102745893A discloses a composite phosphor luminescent glass. The composite phosphor luminescent glass comprises phosphorus-zinc-silicon system glass powder and phosphor. This composite phosphor phosphorus-zinc-silicon luminescent glass contains a high content of ZnO. Preparation of the composite phosphor luminescent glass requires mixing and sintering the glass powder and phosphor. This leads to a strong interfacial reaction between the glass powder and the phosphor, reducing the phosphor's luminous efficiency.

[0005] CN104193346A discloses a translucent phosphor / glass composite luminescent ceramic sheet. The low-melting-point glass powder in this composite luminescent ceramic sheet contains elements such as boron, bismuth, tin, and zinc. This low-melting-point glass powder is mixed with a binder and granulated with the phosphor, followed by molding and sintering. During the sintering process, strong interfacial reactions occur between the glass powder and the phosphor, reducing the phosphor's luminous efficiency.

[0006] CN115893858A discloses a fluorescent glass-ceramic. The fluorescent glass-ceramic comprises a glass matrix, phosphor powder, and a thermally conductive filler. The molar percentages of the glass matrix raw materials are as follows: SiO2: 5-20%, B2O3: 10-35%, ZnO: 20-65%, P2O5: 0.3-15%, and R2O: 0.1-15%, where R2O is at least one of Li2O, Na2O, and K2O, or a combination thereof. The fluorescent glass-ceramic raw materials contain B2O3, and during the preparation process, the glass powder, phosphor powder, and thermally conductive filler are mixed and then sintered in an air atmosphere. During the sintering process, strong interfacial reactions occur between the glass powder and the phosphor powder, resulting in a reduction in the phosphor powder's luminous efficiency. Summary of the Invention

[0007] In view of this, one object of the present invention is to provide a yellow fluorescent glass that can produce white light with high luminous efficiency when excited by blue light. Another object of the present invention is to provide a method for preparing the yellow fluorescent glass. Another object of the present invention is to provide uses of the yellow fluorescent glass. Another object of the present invention is to provide a white light LED light source assembly. Another object of the present invention is to provide a white light LED device.

[0008] The present invention adopts the following technical solutions to achieve the above-mentioned purpose.

[0009] In one aspect, the present invention provides a yellow fluorescent glass, wherein raw materials of the yellow fluorescent glass include glass powder and yellow fluorescent powder, wherein the weight of the yellow fluorescent powder is 22 to 60 wt % of the weight of the glass powder;

[0010] The glass powder is formed by the following components in terms of molar percentage:

[0011] SiO2: 5-15 mol%, P2O5: 20-30 mol%, Al2O3: 35-45 mol%, Na2O: 15-25 mol% and K2O: 1-10 mol%.

[0012] According to the yellow fluorescent glass of the present invention, preferably, the yellow fluorescent powder is YAG:Ce yellow fluorescent powder.

[0013] On the other hand, the present invention also provides a method for preparing the yellow fluorescent glass, comprising the following steps:

[0014] 1) mixing the raw materials of the glass powder according to a proportion to obtain a mixture; ball-milling the mixture to obtain a mixed slurry;

[0015] 2) drying the mixed slurry, and then passing it through a 100-300 mesh sieve to collect the sieved powder to obtain a glass precursor;

[0016] 3) sintering the glass precursor at 1000-2000° C. to obtain a glass melt; quenching the glass melt to obtain a glass solid;

[0017] 4) ball-milling the solidified glass to obtain a coarse glass powder; passing the coarse glass powder through a sieve of 800 to 1200 mesh, collecting the undersize powder to obtain glass powder;

[0018] 5) Sintering the glass powder at 600-800°C to obtain glass liquid;

[0019] 6) The glass liquid is moved to a heating platform at 300-600° C., and then yellow fluorescent powder is added to the glass liquid, stirred, and cooled to obtain yellow fluorescent glass.

[0020] According to the preparation method of the present invention, preferably, in step 1), the rotation speed of the ball mill is 100 to 500 r / min, and the ball milling time is 10 to 20 h.

[0021] According to the preparation method of the present invention, preferably, in step 2), the drying temperature is 50 to 120° C., and the drying time is 12 to 36 hours.

[0022] According to the preparation method of the present invention, preferably, in step 3), the quenching is performed in water.

[0023] According to the preparation method of the present invention, preferably:

[0024] In step 3), the sintering time is 0.5 to 4 hours;

[0025] In step 5), the sintering time is 10 to 60 minutes;

[0026] In step 6), the stirring time is 5 to 30 seconds.

[0027] On the other hand, the present invention also provides a use of the above-mentioned yellow fluorescent glass in white light LEDs, wherein the yellow fluorescent glass emits white light under the excitation of blue light, with a luminous efficiency of at least 147 lm / W and a color temperature of the white light of 4000-5000K.

[0028] In yet another aspect, the present invention further provides a white light LED light source assembly, comprising the above-mentioned yellow fluorescent glass and a blue light LED chip.

[0029] In yet another aspect, the present invention further provides a white light LED device, comprising the above-mentioned white light LED light source assembly.

[0030] The yellow fluorescent glass of the present invention produces white light with high luminous efficiency and moderate color temperature under blue light excitation, which is beneficial for energy saving and extending the life of the lamp. The luminous efficiency of the white light is at least 147lm / W and the color temperature is 4000-5000K. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 1 and 2 are XRD patterns of the yellow fluorescent glass of Example 1 and Comparative Example 1.

[0032] Figure 2 Graphs showing the excitation and emission spectra of the yellow fluorescent glasses of Examples 1 to 3 and Comparative Examples 2 to 3.

[0033] Figure 3 1 is a comparison chart of the excitation spectrum and emission spectrum of the yellow fluorescent glass of Example 1 and Comparative Example 1.

[0034] Figure 4 This is the electroluminescence spectrum of the yellow fluorescent glass of Example 1 under blue light excitation. DETAILED DESCRIPTION

[0035] The present invention will be further described below with reference to specific embodiments, but the protection scope of the present invention is not limited thereto.

[0036] The "luminous efficiency" mentioned in the present invention is the ratio of the luminous flux emitted by a light source to the electrical power consumed, and the unit is lumen / watt (lm / W).

[0037] The "color temperature" mentioned in the present invention refers to the temperature at which a black body is heated to emit light of the same color as the light emitted by a certain light source. The temperature at which the black body is heated is called the color temperature of the light source, abbreviated as color temperature, and the unit is Kelvin (K).

[0038] <Yellow fluorescent glass>

[0039] The yellow fluorescent glass of this invention can be used in blue-light-excited white LEDs, producing white light with high luminous efficiency and a moderate color temperature, making it suitable for solid-state lighting applications. Compared to existing technologies, the yellow fluorescent glass of this invention offers higher luminous efficiency, contributing to energy savings and extended lamp life.

[0040] The yellow fluorescent glass of the present invention comprises glass powder and yellow fluorescent powder.

[0041] According to one embodiment of the present invention, the weight of the yellow phosphor can be 22-60 wt % of the weight of the glass frit, preferably 24-58 wt %, and more preferably 25-55 wt %. Limiting the ratio of the yellow phosphor to the glass frit to the above range is beneficial to improving the luminous efficiency of the yellow fluorescent glass.

[0042] In the present invention, the yellow phosphor can be any commercially available yellow phosphor known in the art, which will not be described in detail here. According to a preferred embodiment of the present invention, the yellow phosphor can be YAG:Ce yellow phosphor, with a chemical composition of Y3Al5O 12 :Ce 3+ .

[0043] According to one embodiment of the present invention, the glass powder is formed by the following components in terms of mole percentage:

[0044] SiO2: 5-15 mol%, P2O5: 20-30 mol%, Al2O3: 35-45 mol%, Na2O: 15-25 mol% and K2O: 1-10 mol%.

[0045] In the glass frit of the present invention, the amount of SiO2 can be 5 to 15 mol%, preferably 6 to 14 mol%, and more preferably 8 to 12 mol%. The amount of P2O5 can be 20 to 30 mol%, preferably 22 to 28 mol%, and more preferably 23 to 26 mol%. The amount of Al2O3 can be 35 to 45 mol%, preferably 36 to 44 mol%, and more preferably 38 to 42 mol%. The amount of Na2O can be 15 to 25 mol%, preferably 16 to 24 mol%, and more preferably 18 to 22 mol%. The amount of K2O can be 1 to 10 mol%, preferably 2 to 8 mol%, and more preferably 3 to 7 mol%.

[0046] Limiting the raw material ratio of glass powder to the above range can ensure that the prepared glass remains liquid at a relatively low temperature after melting, thereby achieving the production of yellow fluorescent glass under low-temperature stirring, which is beneficial to improving the luminous efficiency of the yellow fluorescent glass.

[0047] The raw materials used in the present invention can be commercially available products or prepared by existing preparation methods, which will not be described in detail here. The purity of the raw materials of the present invention is at least industrial purity (99.9 wt%).

[0048] <Preparation method>

[0049] The preparation method of the yellow fluorescent glass includes a mixing and ball milling step, a drying and powder screening step, a primary sintering step, a glass powder preparation step, a secondary sintering step, and a low-temperature stirring reaction step, which is described in detail below.

[0050] Mixing ball milling steps

[0051] The raw materials of the glass powder are mixed according to a proportion to obtain a mixture; and the mixture is ball-milled to obtain a mixed slurry.

[0052] According to one embodiment of the present invention, the ball milling speed may be 100-500 r / min, preferably 120-450 r / min, more preferably 150-400 r / min. The ball milling time may be 10-20 h, preferably 12-20 h, more preferably 12-18 h.

[0053] In the present invention, ball milling can be performed using any type of ball mill known in the art, which will not be described in detail here. For example, a planetary ball mill can be used. The ball milling beads used in the ball milling can be any type known in the art, which will not be described in detail here, but preferably can be Al2O3 balls. The amount of ball milling beads used can be 2 to 8 times the weight of the mixed material, preferably 3 to 8 times, and more preferably 3 to 6 times.

[0054] According to one embodiment of the present invention, anhydrous ethanol may be used as the ball milling medium. The amount of anhydrous ethanol used may be 1.5 to 4 times the mass of the mixture, preferably 1.5 to 3 times, and more preferably 2 to 3 times.

[0055] Reasonable ball milling conditions are conducive to particle refinement, enhancing the reactivity of particles, optimizing sintering performance, and improving the luminous efficiency of yellow fluorescent glass.

[0056] Drying and sieving steps

[0057] The mixed slurry is dried and then passed through a 100-300 mesh sieve to collect the powder under the sieve to obtain a glass precursor.

[0058] According to one embodiment of the present invention, the drying temperature may be 50-120° C., preferably 55-110° C., more preferably 60-100° C. The drying time may be 12-36 h, preferably 15-32 h, more preferably 18-28 h.

[0059] In the present invention, drying can be achieved in any type of drying equipment known in the art, which will not be described in detail herein. For example, a drying oven or an oven can be used.

[0060] According to one embodiment of the present invention, the mesh size of the sieve may be 100 to 300 meshes, preferably 150 to 300 meshes, and more preferably 150 to 250 meshes.

[0061] One sintering step

[0062] The glass precursor is sintered at 1000-2000° C. to obtain a glass melt; the glass melt is quenched to obtain a glass solid.

[0063] According to one embodiment of the present invention, the temperature is raised from room temperature (25°C, the same below) to the sintering temperature at a rate of 5-20°C / min, preferably 5-15°C / min, and more preferably 10-15°C / min. The sintering temperature may be 1000-2000°C, preferably 1100-1800°C, and more preferably 1200-1600°C. The sintering time may be 0.5-4 hours, preferably 1-4 hours, and more preferably 1-3 hours.

[0064] In the present invention, quenching can be carried out in any quenching medium known in the art, which will not be described in detail herein. For example, quenching can be carried out in water, preferably deionized water.

[0065] In the present invention, sintering can be performed in any sintering device known in the art, which will not be described in detail here, for example, a high-temperature sintering furnace, a muffle furnace, etc.

[0066] Reasonable sintering conditions can ensure that the prepared glass remains liquid at a relatively low temperature after melting, thereby achieving the production of yellow fluorescent glass under low-temperature stirring, which is beneficial to improving the luminous efficiency of the yellow fluorescent glass.

[0067] Glass powder preparation steps

[0068] The glass solid is ball-milled to obtain coarse glass powder; the coarse glass powder is passed through a sieve of 800 to 1200 meshes, and the powder under the sieve is collected to obtain glass powder.

[0069] According to one embodiment of the present invention, the mesh size of the sieve may be 800-1200 meshes, preferably 850-1150 meshes, and more preferably 900-1100 meshes.

[0070] Ball milling can be achieved using any type of ball mill known in the art, which will not be described in detail here. For example, a planetary ball mill can be used. The ball milling beads used in the ball milling can be of any type known in the art, which will not be described in detail here, and preferably can be Al2O3 balls. The amount of ball milling beads used can be 2 to 8 times the weight of the mixture, preferably 3 to 8 times, and more preferably 3 to 6 times. Anhydrous ethanol can be used as the ball milling medium, and the amount of anhydrous ethanol used can be 1.5 to 4 times the mass of the mixture, preferably 1.5 to 3 times, and more preferably 2 to 3 times.

[0071] According to a preferred embodiment of the present invention, the process may further include drying the milled glass slurry to obtain a coarse glass powder. The drying temperature may be 50-120°C, preferably 55-110°C, and more preferably 60-100°C. The drying time may be 12-36 hours, preferably 15-32 hours, and more preferably 18-28 hours. Drying may be performed using any type of drying equipment known in the art and will not be described in detail herein.

[0072] Secondary sintering step

[0073] The glass powder is sintered at 600-800°C to obtain glass liquid.

[0074] According to one embodiment of the present invention, the temperature is raised from room temperature to the sintering temperature at a rate of 5-20°C / min, preferably 5-15°C / min, and more preferably 10-15°C / min. The sintering temperature may be 600-800°C, preferably 620-780°C, and more preferably 650-750°C. The sintering time may be 10-60 minutes, preferably 10-50 minutes, and more preferably 15-50 minutes.

[0075] Reasonable sintering conditions can ensure that the prepared glass liquid is stirred and mixed with the yellow phosphor at a lower temperature, which is beneficial to improving the luminous efficiency of the yellow fluorescent glass.

[0076] Low temperature stirring reaction step

[0077] The glass liquid is moved to a heating platform at 300-600°C, and then yellow fluorescent powder is added to the glass liquid, stirred, and cooled to obtain yellow fluorescent glass.

[0078] According to one embodiment of the present invention, the temperature of the heating stage may be 300-600°C, preferably 320-580°C, and more preferably 350-550°C.

[0079] In the present invention, the heating platform can be any type of constant temperature heating platform known in the art, which will not be described in detail here.

[0080] In the present invention, stirring can be achieved using any stirring equipment known in the art, which will not be described in detail here.

[0081] According to one embodiment of the present invention, the stirring time may be 5 to 30 s, preferably 6 to 20 s, and more preferably 8 to 15 s.

[0082] Reasonable temperature and stirring conditions can ensure that the yellow fluorescent powder retains better activity in the glass liquid. The obtained yellow fluorescent glass has a uniform microstructure and an ideal crystal phase, which is beneficial to improving the luminous efficiency of the yellow fluorescent glass.

[0083] In the present invention, cooling can be achieved by any cooling method known in the art, which will not be described in detail here. For example, it can be natural cooling or air cooling.

[0084] <Purpose>

[0085] The present invention also provides use of the yellow fluorescent glass in white light LEDs.

[0086] According to one embodiment of the present invention, yellow fluorescent glass emits white light when excited by blue light. The luminous efficiency can be at least 147 lm / W, preferably at least 147.5 lm / W, and more preferably at least 147.8 lm / W. The color temperature of the white light can be between 4000 and 5000K, preferably between 4050 and 4900K, and more preferably between 4100 and 4880K.

[0087] <White LED light source component>

[0088] The present invention also provides a white light LED light source assembly, comprising the yellow fluorescent glass and a blue light LED chip.

[0089] According to one embodiment of the present invention, the wavelength of the blue LED chip may be 400-495 nm, preferably 420-490 nm, more preferably 450-470 nm, and most preferably 455 nm.

[0090] According to one embodiment of the present invention, the yellow fluorescent glass can be manufactured into any shape and specification according to actual needs, which will not be further described here. According to a preferred embodiment of the present invention, the yellow fluorescent glass can be in the form of a disc. The bottom diameter of the disc can be 10 to 30 mm, preferably 15 to 30 mm, and more preferably 15 to 25 mm. The thickness of the disc can be 0.2 to 1 mm, preferably 0.2 to 0.8 mm, and more preferably 0.3 to 0.8 mm.

[0091] <White LED Devices>

[0092] The present invention also provides a white light LED device, comprising the above-mentioned white light LED light source assembly.

[0093] <Test method>

[0094] XRD detection: The X'Pert PRO XRD powder diffractometer produced by Panalytical was used for determination.

[0095] Excitation and emission spectra were measured using an FSL1000 steady-state / transient fluorescence spectrometer produced by Edinburgh Instruments.

[0096] Luminous efficiency, color temperature and electroluminescence spectrum detection: Use the PCE-2000A photoelectric color comprehensive test system produced by Hangzhou Yuanfang Optoelectronic Information Co., Ltd.

[0097] <Ingredients>

[0098] Unless otherwise specified, the raw materials in the following examples are all commercially available products.

[0099] Among them, Y3Al5O 12 :Ce 3+ Yellow phosphor was purchased from Beijing Zhongcun Yuji Technology Co., Ltd.

[0100] Example 1

[0101] The glass powder is composed of the following components, measured in molar percentages: SiO2: 10 mol, P2O5: 25 mol, Al2O3: 40 mol, Na2O: 20 mol, and K2O: 5 mol. The yellow fluorescent glass is prepared using the following steps:

[0102] The raw materials of the glass powder are mixed according to a proportion to obtain a mixture; the mixture is placed in a star ball mill, and Al2O3 balls with a weight that is 5 times the weight of the mixture are added as ball milling beads, followed by adding anhydrous ethanol with a weight that is 2 times the weight of the mixture, and ball milling is carried out at a speed of 200 r / min for 16 hours to obtain a mixed slurry.

[0103] The mixed slurry was placed in an evaporating dish and dried at 80°C for 24 hours to obtain a dried powder. The dried powder was then passed through a 200-mesh sieve and the undersize powder was collected to obtain a glass precursor.

[0104] The glass precursor is placed in a muffle furnace and sintered at 1300° C. for 2 hours to melt the glass precursor to obtain a glass melt. The glass melt is placed in deionized water for quenching to obtain a glass solid.

[0105] The solidified glass was placed in a planetary ball mill, and Al2O3 balls were added as milling beads at a weight of 5 times the weight of the solidified glass. Anhydrous ethanol was then added at a weight of 2 times the weight of the solidified glass. The mill was milled at 200 r / min for 16 hours to obtain a glass slurry. The glass slurry was placed in an evaporating dish and dried at 80°C for 24 hours to obtain a coarse glass powder. The coarse glass powder was passed through a 1000-mesh sieve, and the undersize powder was collected to obtain glass powder.

[0106] The glass powder was placed in a crucible, and the crucible was placed in a muffle furnace. The temperature was raised from room temperature to 700°C at a rate of 10°C / min, and the crucible was sintered at 700°C for 20 minutes to obtain glass liquid.

[0107] The crucible containing the glass liquid was placed on a heating platform at 400 °C, and Y3Al5O 12 :Ce 3+ Yellow fluorescent powder was added into the glass liquid, stirred for 10 seconds, and then naturally cooled to obtain yellow fluorescent glass.

[0108] Example 2

[0109] The only difference from Example 1 is that 30 wt% of the weight of the glass powder is added to the Y3Al5O 12 :Ce 3+ Yellow phosphor is added to the glass liquid.

[0110] Example 3

[0111] The only difference from Example 1 is that the weight of Y3Al5O is 50 wt% of the weight of the glass powder. 12 :Ce 3+ Yellow phosphor is added to the glass liquid.

[0112] Comparative Example 1

[0113] Except for the following parameters and settings, the rest are the same as Example 1:

[0114] The glass powder was mixed with 40 wt% of Y3Al5O 12 :Ce 3+ The yellow phosphor powders are mixed and placed in a crucible, which is then placed in a muffle furnace and heated from room temperature to 700°C at a rate of 10°C / min. The crucible is sintered at 700°C for 20 minutes to obtain a yellow fluorescent glass liquid, which is then naturally cooled to obtain a yellow fluorescent glass.

[0115] Comparative Example 2

[0116] The only difference from Example 1 is that 10 wt% of the weight of the glass powder is added to the Y3Al5O 12 :Ce 3+ Yellow phosphor is added to the glass liquid.

[0117] Comparative Example 3

[0118] The only difference from Example 1 is that 20 wt% of the weight of the glass powder is added to the Y3Al5O 12 :Ce 3+ Yellow phosphor is added to the glass liquid.

[0119] Experimental Example 1

[0120] The yellow fluorescent glass prepared in Example 1 and the yellow fluorescent glass prepared in Comparative Example 1 were cut into disc samples with a bottom diameter of 20 mm and a thickness of 0.5 mm, and then the surfaces of the samples were polished to make them smooth to prepare test samples. The test sample of the yellow fluorescent glass prepared in Example 1 (denoted as Example 1), the test sample of the yellow fluorescent glass prepared in Comparative Example 1 (denoted as Comparative Example 1), the glass powder prepared in Example 1 (denoted as glass powder), and Y3Al5O 12 :Ce 3+ The yellow phosphor (denoted as YAG:Ce) was tested by XRD (X-ray diffraction), and the results were as follows Figure 1 shown.

[0121] Depend on Figure 1 It can be seen that the yellow fluorescent glass prepared in Example 1, the yellow fluorescent glass prepared in Comparative Example 1 and the Y3Al5O 12 :Ce 3+ The diffraction peaks of the XRD pattern of the yellow phosphor are sharp, and the peak positions correspond to the diffraction peaks identified by the standard PDF card JCPDS 33-0040, indicating that the yellow phosphor glass prepared in Example 1 retains a complete yellow phosphor crystal phase.

[0122] Experimental Example 2

[0123] The yellow fluorescent glasses prepared in Examples 1 to 3 and Comparative Examples 1 to 3 were cut into disc samples with a bottom diameter of 20 mm and a thickness of 0.5 mm, and then the surfaces of the samples were polished to make the surfaces smooth to prepare test samples. The excitation spectrum and emission spectrum of the test samples of the yellow fluorescent glasses prepared in Examples 1 to 3 (respectively referred to as Examples 1 to 3) and the test samples of the yellow fluorescent glasses prepared in Comparative Examples 1 to 3 (respectively referred to as Comparative Examples 1 to 3) were tested, and the results are as follows: Figure 2 and 3 shown.

[0124] Depend on Figure 2 and 3 As can be seen, the yellow fluorescent glasses produced in Examples 1-3 and Comparative Examples 1-3 all exhibit strong emission in the 555nm band under 455nm blue light excitation, and all samples maintain the luminescence characteristics of the phosphor. This demonstrates that the yellow fluorescent glasses produced in Examples 1-3 and Comparative Examples 1-3 can emit yellow light under blue light excitation, and that the low-temperature stirring process of the present invention can better maintain the luminescence characteristics of the phosphor. The intensity of the yellow light emitted by the yellow fluorescent glass produced in the present invention is significantly stronger than that of the comparative examples.

[0125] Application Experiment Example 1

[0126] Test samples of yellow fluorescent glass prepared in Examples 1-3 of Experimental Example 3 (referred to as Examples 1-3) and test samples of yellow fluorescent glass prepared in Comparative Examples 1-3 (referred to as Comparative Examples 1-3) were packaged onto 455nm blue LED chips to produce white light LED light source assemblies. White light LED devices were then fabricated using the white light LED light source assemblies. Under excitation from the 455nm blue LED chips, the yellow fluorescent glass exhibited white light emission. The color temperature and luminous efficiency of the test samples are shown in Table 1.

[0127] Table 1

[0128] Test samples Luminous efficiency (lm / W) Color temperature (K) Example 1 154.88 4363 Example 2 147.88 4865 Example 3 148.43 4114 Comparative Example 1 144.28 4561 Comparative Example 2 117.92 5663 Comparative Example 3 127.85 5214

[0129] As can be seen from Table 1, the white light obtained by the yellow fluorescent glass of the present invention has a moderate color temperature and a luminous intensity significantly higher than that of the comparative example.

[0130] The electroluminescence spectrum of the yellow fluorescent glass sample prepared in Example 1 was tested. The results are as follows: Figure 4 As shown. Figure 4 It can be seen that the yellow fluorescent glass of the present invention has strong yellow light emission, indicating that it has excellent light conversion ability.

[0131] The present invention is not limited to the above-mentioned embodiments. Any modification, improvement, or substitution that can be conceived by those skilled in the art without departing from the essential content of the present invention shall fall within the scope of the present invention.

Claims

1. A yellow fluorescent glass, characterized in that: The raw materials of the yellow fluorescent glass include glass powder and yellow fluorescent powder, and the weight of the yellow fluorescent powder is 22-60wt% of the weight of the glass powder; The glass powder is formed by the following components in terms of molar percentage: SiO2: 5-15 mol%, P2O5: 20-30 mol%, Al2O3: 35-45 mol%, Na2O: 15-25 mol% and K2O: 1-10 mol%.

2. The yellow fluorescent glass according to claim 1, characterized in that: The yellow phosphor is YAG:Ce yellow phosphor.

3. A method for preparing the yellow fluorescent glass according to claim 1 or 2, characterized in that: The following steps are involved: 1) mixing the raw materials of the glass powder according to a proportion to obtain a mixture; ball-milling the mixture to obtain a mixed slurry; 2) drying the mixed slurry, and then passing it through a 100-300 mesh sieve to collect the sieved powder to obtain a glass precursor; 3) sintering the glass precursor at 1000-2000° C. to obtain a glass melt; quenching the glass melt to obtain a glass solid; 4) ball-milling the solidified glass to obtain a coarse glass powder; passing the coarse glass powder through a sieve of 800 to 1200 mesh, collecting the undersize powder to obtain glass powder; 5) Sintering the glass powder at 600-800°C to obtain glass liquid; 6) The glass liquid is moved to a heating platform at 300-600° C., and then yellow fluorescent powder is added to the glass liquid, stirred, and cooled to obtain yellow fluorescent glass.

4. The preparation method according to claim 3, characterized in that In step 1), the ball milling speed is 100 to 500 r / min, and the ball milling time is 10 to 20 hours.

5. The preparation method according to claim 3, characterized in that In step 2), the drying temperature is 50 to 120° C., and the drying time is 12 to 36 hours.

6. The preparation method according to claim 3, characterized in that In step 3), the quenching is carried out in water.

7. The preparation method according to claim 3, wherein: In step 3), the sintering time is 0.5 to 4 hours; In step 5), the sintering time is 10 to 60 minutes; In step 6), the stirring time is 5 to 30 seconds.

8. Use of the yellow fluorescent glass according to claim 1 or 2 in a white light LED, characterized in that: The yellow fluorescent glass emits white light under the excitation of blue light, with a luminous efficiency of at least 147 lm / W and a color temperature of the white light of 4000-5000K.

9. A white light LED light source assembly, characterized in that: The white light LED light source assembly comprises the yellow fluorescent glass according to claim 1 or 2 and a blue light LED chip.

10. A white light LED device, characterized in that: The white light LED device includes the white light LED light source assembly according to claim 9.

Citation Information

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