Optoelectronic glass, its preparation method, and light-emitting device

Abstract

This application relates to the field of laser lighting technology, and relates to an optoelectronic glass, a preparation method thereof, and a light-emitting device. The optoelectronic glass includes: light-emitting points and a matrix; the light-emitting points are dispersed in the matrix; the light-emitting points are graphene quantum dot materials, and the matrix is an aluminoborosilicate-based glass-ceramic. In the optoelectronic glass of this application, the graphene quantum dots are uniformly dispersed in the glass-ceramic matrix without agglomeration, which helps to improve the luminous efficiency and luminous uniformity of high-power white light lighting devices. Moreover, compared with the existing light-emitting thin films, the optoelectronic glass of this application can exhibit more excellent mechanical strength, thermal stability, and corrosion resistance. Therefore, applying the novel optoelectronic glass of this application to a light-emitting device can improve the luminous stability of the device and solve problems such as light flux attenuation, stability degradation, and color coordinate drift in polymer light-emitting devices.

Description

Technical Field

[0001] This application relates to the technical field of laser lighting, and in particular, to an optoelectronic glass, a preparation method thereof, and a light-emitting device. Background Art

[0002] With the increasing demand for high-brightness lighting by people, semiconductor white solid-state lighting is gradually developing towards high excitation density and high stability. White lighting based on laser diodes (LDs) has been widely used in high-power solid-state lighting fields such as vehicle headlights, cinema projection lights, tunnel lights, and sea-sweeping lights due to its many characteristics such as high brightness, long range, low power consumption, and long lifespan.

[0003] As a new generation of optoelectronic functional materials, graphene quantum dots (GQDs) have advantages such as high fluorescence yield, good optical stability, high chemical stability, and adjustable emission spectrum. However, liquid-phase synthesized GQDs exhibit serious fluorescence quenching phenomena in the solid state due to strong π-π stacking between each other, which greatly limits their potential applications in LD light conversion materials.

[0004] To overcome this obstacle, currently, researchers have compounded GQDs into organic polymers to obtain light-emitting films. However, due to the low thermal conductivity and poor thermal stability of the polymer matrix, the traditional encapsulation method of "light-emitting material + organic material" makes LDs generally have aging and yellowing phenomena, which in turn leads to problems such as light flux attenuation, stability decline, and color coordinate drift of the devices. Summary of the Invention

[0005] The purpose of the embodiments of this application is to provide an optoelectronic glass, a preparation method thereof, and a light-emitting device.

[0006] In a first aspect, this application provides an optoelectronic glass, including:

[0007] Light-emitting points and a matrix; the light-emitting points are dispersed in the matrix;

[0008] The light-emitting points are graphene quantum dot materials, and the matrix is an aluminoborosilicate-based glass-ceramic.

[0009] In this application, a novel optoelectronic glass is obtained by compounding graphene quantum dot materials with aluminoborosilicate microcrystalline glass. On the one hand, in this novel optoelectronic glass, the graphene quantum dots are uniformly dispersed and non-aggregated in the microcrystalline glass matrix, which helps to improve the luminous efficiency and luminous uniformity of high-power white lighting devices. On the other hand, compared with the existing light-emitting thin films (i.e., the matrix material is replaced by inorganic microcrystalline glass instead of organic polymer), this novel optoelectronic glass can exhibit more excellent mechanical strength, thermal stability, and corrosion resistance. Based on the above two aspects, applying the novel optoelectronic glass of this application to light-emitting devices can improve the luminous stability of the devices and solve problems such as light flux attenuation, stability decline, and color coordinate drift that occur in polymer light-emitting devices.

[0010] In other embodiments of this application, in terms of mass percentage, the mass of the light-emitting points is 20% - 40% of the matrix.

[0011] In other embodiments of this application, the above-mentioned graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots; among them, the carbon source of the graphene quantum dots is fullerene;

[0012] The modified graphene quantum dots are 2,3-diaminonaphthalene-modified graphene quantum dots.

[0013] In other embodiments of this application, in the above-mentioned graphene quantum dot material, the volume ratio of graphene quantum dots to modified graphene quantum dots is 0.5:1 - 2:1.

[0014] In other embodiments of this application, the emission wavelength of the above-mentioned graphene quantum dot material is 400nm - 700nm.

[0015] In other embodiments of this application, the thickness of the above-mentioned optoelectronic glass is 1.35mm - 2.35mm.

[0016] In other embodiments of this application, the above-mentioned aluminoborosilicate microcrystalline glass is an Al2O3 - B2O3 - SiO2 - ZnO system.

[0017] In other embodiments of this application, the above-mentioned aluminoborosilicate microcrystalline glass includes: 5mol% - 20mol% alumina, 40mol% - 60mol% boric oxide, 25mol% - 45mol% silica, and 0mol% - 10mol% zinc oxide.

[0018] Second, this application provides a preparation method of an optoelectronic glass, including:

[0019] After uniformly mixing the graphene quantum dot material with the aluminoborosilicate microcrystalline glass powder, keep it at 650°C - 750°C for 0.5h - 1.5h.

[0020] In other embodiments of the present application, the above-mentioned graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots;

[0021] Preparing graphene quantum dots includes:

[0022] Mixing a fullerene and potassium peroxymonosulfate solution, reacting at 140°C to 200°C for 2h to 14h; then making the obtained reactant into a powder.

[0023] In other embodiments of the present application, preparing modified graphene quantum dots includes:

[0024] Mixing graphene quantum dots and 2,3-diaminonaphthalene evenly, then reacting at 170°C to 190°C for 12h to 15h, and making the reactant into a powder.

[0025] In a third aspect, the present application provides a light-emitting device, including: the optoelectronic glass of any one of the foregoing; or the optoelectronic glass prepared by the preparation method of the foregoing optoelectronic glass. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] To more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings required for the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and thus should not be regarded as limiting the scope. For those of ordinary skill in the art, other related drawings can also be obtained based on these drawings without creative efforts.

[0027] Figure 1 It is the transmission electron microscope imaging diagram of the optoelectronic glass prepared in the embodiment of the present application;

[0028] Figure 2 It is the transmittance spectrum diagram of the optoelectronic glass prepared in the embodiment of the present application;

[0029] Figure 3 It is the PL spectrum and CIE 1931 color coordinates of the optoelectronic glass prepared in the embodiment of the present application under 385nm laser irradiation;

[0030] Figure 4 It is the light emission intensity diagram of the optoelectronic glass prepared in the embodiment of the present application after heating-cooling cycles in the range from room temperature to 320°C;

[0031] Figure 5 It is the light emission intensity angular distribution diagram of the laser illumination device of the optoelectronic glass prepared in the embodiment of the present application;

[0032] Figure 6 It is the emission intensity (driving current is 1200mA) of the laser illumination device of the optoelectronic glass prepared in the embodiment of the present application at different working times. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0033] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below. Apparently, the described embodiments are some but not all of the embodiments of this application.

[0034] Therefore, the following detailed description of the embodiments of this application is not intended to limit the scope of this application that is claimed, but merely represents selected embodiments of this application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in this application without creative efforts fall within the scope of protection of this application.

[0035] An optoelectronic glass is provided in an embodiment of this application, including:

[0036] Light-emitting points and a matrix; the light-emitting points are dispersed in the matrix;

[0037] The light-emitting points are graphene quantum dot materials, and the matrix is an aluminoborosilicate-based glass-ceramic.

[0038] For the optoelectronic glass provided in the embodiment of this application, on the one hand, as a matrix material, the aluminoborosilicate-based glass-ceramic can retain the light-emitting characteristics of the graphene quantum dot material and can withstand high-density laser irradiation under high-temperature and high-humidity conditions without deformation. Therefore, compared with existing light-emitting films (i.e., the matrix material is replaced by inorganic glass-ceramics instead of organic polymers), the optoelectronic glass of this application exhibits excellent mechanical strength, thermal stability, and corrosion resistance.

[0039] On the other hand, for the optoelectronic glass provided in the embodiment of this application, the graphene quantum dot material is combined with the aluminoborosilicate-based glass-ceramic to obtain a new type of optoelectronic glass. Among them, the graphene quantum dot material serves as the light-emitting center, and the aluminoborosilicate-based glass-ceramic serves as the matrix material. A large number of graphene quantum dot materials are evenly distributed in the aluminoborosilicate-based glass-ceramic matrix without agglomeration, which will help improve the light-emitting efficiency and light-emitting uniformity of high-power white-light lighting devices.

[0040] Based on the above two aspects, it can be concluded that the optoelectronic glass prepared in this application is applied to a light-emitting device, which can improve the light-emitting stability of the device and solve problems such as light flux attenuation, stability decline, and color coordinate drift that occur in polymer light-emitting devices. Further, in some embodiments of this application, by mass percentage, the mass of the light-emitting points is 20% to 40% of the matrix.

[0041] Further optionally, by mass percentage, the mass of the light-emitting points is 21% to 39% of the matrix. Exemplarily, the mass of the light-emitting points is 22%, 25%, 28%, 30%, 32%, 35%, or 38% of the matrix.

[0042] Further, in some embodiments of the present application, the above-mentioned graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots; wherein, the carbon source of the graphene quantum dots is fullerene.

[0043] Further, in some embodiments of the present application, the above-mentioned modified graphene quantum dots are 2,3-diaminonaphthalene modified graphene quantum dots.

[0044] Further, in some embodiments of the present application, in the above-mentioned graphene quantum dot material, the volume ratio of graphene quantum dots to modified graphene quantum dots is 0.5:1 to 2:1.

[0045] Further optionally, in some embodiments of the present application, in the above-mentioned graphene quantum dot material, the volume ratio of graphene quantum dots to modified graphene quantum dots is 0.6:1 to 1.9:1.

[0046] Exemplarily, in the above-mentioned graphene quantum dot material, the volume ratio of graphene quantum dots to modified graphene quantum dots is 0.7:1, 0.8:1, 0.9:1, 1.0:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1 or 1.8:1.

[0047] Further, in some embodiments of the present application, the emission wavelength of the graphene quantum dot material is 400 nm to 700 nm.

[0048] Further optionally, the emission wavelength of the graphene quantum dot material is 410 nm to 690 nm.

[0049] Exemplarily, the emission wavelength of the graphene quantum dot material is 450 nm, 480 nm, 500 nm, 520 nm, 550 nm, 580 nm, 600 nm, 620 nm, 650 nm or 680 nm.

[0050] Further, in some embodiments of the present application, the thickness of the optoelectronic glass is 1.35 mm to 2.35 mm.

[0051] Further optionally, the thickness of the optoelectronic glass is 1.4 mm to 2.3 mm. Exemplarily, the thickness of the optoelectronic glass is 1.5 mm, 1.8 mm, 1.9 mm, 2.0 mm or 2.2 mm.

[0052] Further, in some embodiments of the present application, the aluminoborosilicate glass-ceramics is an Al2O3-B2O3-SiO2-ZnO system.

[0053] Further, in some embodiments of the present application, the aluminoborosilicate glass-ceramics include: 5 mol% to 20 mol% of alumina, 40 mol% to 60 mol% of boric oxide, 25 mol% to 45 mol% of silica, and 0 mol% to 10 mol% of zinc oxide.

[0054] Further optionally, the aluminoborosilicate glass-ceramics include: 6 mol% to 19 mol% of alumina, 41 mol% to 59 mol% of boric oxide, 26 mol% to 44 mol% of silica, and 0.5 mol% to 9.5 mol% of zinc oxide.

[0055] Exemplarily, the aluminoborosilicate glass-ceramics include: 5 mol%, 8 mol%, 10 mol%, 12 mol%, 15 mol% or 18 mol% of alumina;

[0056] Exemplarily, the aluminoborosilicate glass-ceramics include: 42 mol%, 45 mol%, 48 mol%, 50 mol%, 52 mol%, 55 mol% or 58 mol% of boric oxide;

[0057] Exemplarily, the aluminoborosilicate glass-ceramics include: 28 mol%, 30 mol%, 32 mol%, 35 mol%, 38 mol%, 40 mol%, 42 mol% or 44 mol% of silica;

[0058] Exemplarily, the aluminoborosilicate glass-ceramics include: 1 mol%, 3 mol%, 5 mol%, 7 mol% or 8 mol% of zinc oxide.

[0059] Some embodiments of the present application provide a method for preparing an optoelectronic glass, including:

[0060] After uniformly mixing the graphene quantum dot material powder and the aluminoborosilicate glass-ceramics powder, keep it at 650 °C to 750 °C for 0.5 h to 1.5 h.

[0061] Further, in some embodiments of the present application, the method for preparing an optoelectronic glass includes the following steps:

[0062] Step S1, prepare the graphene quantum dot material.

[0063] Among them, the graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots; among them, the carbon source of the graphene quantum dots is fullerene.

[0064] The modified graphene quantum dots are 2,3-diaminonaphthalene modified graphene quantum dots.

[0065] In some embodiments of the present application, preparing the graphene quantum dots includes:

[0066] React the mixed solution of fullerene and potassium peroxymonosulfate at 140 °C to 200 °C for 2 h to 14 h; then make the obtained reactant into powder.

[0067] Further optionally, preparing graphene quantum dots includes:

[0068] React the mixed solution of fullerene and potassium peroxymonosulfate at 145 °C to 195 °C for 2.5 h to 13.5 h; then make the obtained reactant into powder.

[0069] Exemplarily, preparing graphene quantum dots includes:

[0070] React the mixed solution of fullerene and potassium peroxymonosulfate at 150 °C, 155 °C, 160 °C, 165 °C, 170 °C, 175 °C, 180 °C, 185 °C, 190 °C for 3 h, 4 h, 5 h, 6 h, 7 h, 8 h, 9 h, 10 h, 11 h, 12 h, 13 h; then make the obtained reactant into powder.

[0071] In some embodiments of the present application, preparing modified graphene quantum dots includes:

[0072] Mix the previously prepared graphene quantum dots with 2,3-diaminonaphthalene evenly, then react at 170 °C to 180 °C for 12 h to 15 h, and make the reactant into powder.

[0073] Further optionally, in some embodiments of the present application, preparing modified graphene quantum dots includes:

[0074] Mix the previously prepared graphene quantum dots with 2,3-diaminonaphthalene evenly, then react at 171 °C to 179 °C for 12.5 h to 14.5 h, and make the reactant into powder.

[0075] Exemplarily, preparing modified graphene quantum dots includes:

[0076] Mix the previously prepared graphene quantum dots with 2,3-diaminonaphthalene evenly, then react at 172 °C, 173 °C, 174 °C, 175 °C, 176 °C, 177 °C, 178 °C for 12.5 h, 13 h, 13.5 h, 14 h or 14.5 h, and make the reactant into powder.

[0077] Further optionally, in some specific embodiments of the present application, preparing the mixed solution of fullerene and potassium peroxymonosulfate includes: dissolving fullerene and potassium peroxymonosulfate in DMF, and ultrasonically treating for 1 h to 3 h to obtain a reaction solution. Exemplarily, dissolve fullerene and potassium peroxymonosulfate in DMF, and ultrasonically treat for 1 h, 1.5 h, 2 h, 2.5 h or 3 h to obtain a reaction solution.

[0078] Further optionally, in some specific embodiments of the present application, the mixed solution of fullerene and potassium peroxymonosulfate is reacted at 140 °C to 200 °C for 2.5 h to 13.5 h, and the obtained reactant is made into powder; including: keeping the above-prepared reaction solution in a reaction kettle at 140 °C to 200 °C for 2 h to 14 h, cooling to room temperature, and finally purifying and drying to obtain graphene quantum dots (GQDs) powder.

[0079] Further optionally, in some specific embodiments of the present application, the modification with 2,3-diaminonaphthalene includes: mixing the above-prepared GQDs with a certain amount of 2,3-diaminonaphthalene, ultrasonically treating for 1 h to 3 h, keeping warm in a reaction kettle at 180 °C for 12 h, and finally purifying and drying to obtain modified graphene quantum dots (M-GQDs) powder.

[0080] It should be noted that single graphene quantum dots (GQDs) mainly emit blue-green fluorescence, while single modified graphene quantum dots (M-GQDs) mainly emit orange-yellow fluorescence. The present application can emit white fluorescence by fully mixing graphene quantum dots (GQDs) and modified graphene quantum dots (M-GQDs).

[0081] Step S2: Prepare aluminoborosilicate glass-ceramic powder.

[0082] In some embodiments of the present application, the preparation of aluminoborosilicate glass-ceramic powder includes: grinding and mixing 5 mol% to 20 mol% of alumina, 40 mol% to 60 mol% of boric oxide, 25 mol% to 45 mol% of silica, and 0 mol% to 10 mol% of zinc oxide evenly, and keeping warm at 1200 °C to 1400 °C for 1 h to 3 h.

[0083] Further optionally, the preparation of aluminoborosilicate glass-ceramic powder includes: grinding and mixing 5.5 mol% to 19.5 mol% of alumina, 45 mol% to 55 mol% of boric oxide, 26 mol% to 44 mol% of silica, and 0.1 mol% to 9.5 mol% of zinc oxide evenly, and keeping warm at 1250 °C to 1350 °C for 1.1 h to 2.9 h.

[0084] Exemplarily, preparing the aluminoborosilicate-based glass-ceramic powder includes: grinding and uniformly mixing 6 mol%, 8 mol%, 10 mol%, 12 mol%, 15 mol%, 18 mol% of alumina, 45 mol%, 48 mol%, 50 mol%, 52 mol%, 54 mol% of boric oxide, 27 mol%, 29 mol%, 32 mol%, 34 mol%, 36 mol%, 38 mol%, 42 mol% of silica, and 0.5 mol%, 2 mol%, 5 mol%, 8 mol%, 9 mol% of zinc oxide, and then holding at 1250 °C, 1280 °C, 1300 °C, 1320 °C, 1340 °C for 1.5 h, 1.8 h, 2 h, 2.5 h, 2.8 h.

[0085] Further optionally, in some specific embodiments of the present application, preparing the aluminoborosilicate-based glass-ceramic powder includes:

[0086] Weigh the required glass matrix raw materials according to the above-designed components, place the weighed raw materials in a mortar, grind and mix them evenly to obtain a mixture. The mixture is placed in a corundum crucible, heated to 1200 °C to 1400 °C and held for 1 h to 3 h, quenched with water to obtain precursor glass slag, and further pulverized to obtain the aluminoborosilicate-based glass-ceramic powder.

[0087] Step S3: Prepare the optoelectronic glass.

[0088] In some embodiments of the present application, preparing the optoelectronic glass includes: uniformly mixing the graphene quantum dot material obtained in step S1 and the aluminoborosilicate-based glass-ceramic powder obtained in step S2, and then holding at 650 °C to 750 °C for 0.5 h to 1.5 h.

[0089] By controlling the above preparation process conditions, a large amount of graphene quantum dot materials can be evenly distributed in the aluminoborosilicate-based glass-ceramic matrix without agglomeration.

[0090] Further, in some embodiments of the present application, in the above graphene quantum dot material, the volume ratio of graphene quantum dots to modified graphene quantum dots is 0.5:1 to 2:1.

[0091] Further optionally, preparing the optoelectronic glass includes: uniformly mixing the graphene quantum dot material obtained in step S1 and the aluminoborosilicate-based glass-ceramic powder obtained in step S2, and then holding at 655 °C to 745 °C for 0.6 h to 1.4 h.

[0092] Exemplarily, the preparation of the optoelectronic glass includes: after uniformly mixing the graphene quantum dot material obtained in step S1 and the aluminoborosilicate-based glass-ceramic powder obtained in step S2, keeping the temperature at 660 °C, 670 °C, 680 °C, 690 °C, 700 °C, 710 °C, 720 °C, 730 °C, 740 °C for 0.6 h, 0.8 h, 0.9 h, 1 h, 1.2 h, 1.3 h.

[0093] In some embodiments of the present application, in some specific embodiments of the present application, the aluminoborosilicate-based glass-ceramic powder prepared in step S2 and the graphene quantum dot material prepared in step S1 (the volume ratio of GQDs to M-GQDs is 0.5:1 to 2:1) are uniformly mixed, and then the mixture is transferred to a mold and cold isostatically pressed to form a green body. Then the green body is heated to 650 °C - 750 °C in an air atmosphere and kept for 0.5 h - 1.5 h to obtain the optoelectronic glass.

[0094] Some embodiments of the present application provide a light-emitting device, including: the optoelectronic glass provided in any one of the foregoing embodiments; or the optoelectronic glass prepared by the preparation method of the optoelectronic glass provided in any one of the foregoing embodiments.

[0095] The features and properties of the present application are further described in detail below in conjunction with the embodiments:

[0096] Example 1

[0097] An optoelectronic glass is provided and prepared according to the following steps:

[0098] 1) Weigh 0.1 g of fullerene and 0.4 g of potassium peroxymonosulfate, add them to 20 mL of DMF, ultrasonically disperse for 1.5 h to obtain a reaction solution, pour the reaction solution into a 50 mL reaction kettle lined with polytetrafluoroethylene, keep the temperature at 160 °C for 7 h, take out the reaction product after the reaction kettle cools, and then centrifuge the reaction product at a speed of 4000 revolutions per minute for 40 minutes to remove the remaining potassium peroxymonosulfate and large residues. Take the supernatant, first filter it with a 0.22 μm filter membrane, and then dialyze it with a semipermeable membrane with a molecular weight cut-off of 3500 Da for three days to obtain a graphene quantum dot (GQDs) solution, and obtain GQDs powder after removing the solvent by rotary evaporation.

[0099] 2) Weigh 5 mL of the GQDs aqueous solution and mix it with 20 mg of 2,3-diaminonaphthalene. Add them to 20 mL of DMF, and ultrasonically disperse for 1.5 h to obtain a reaction solution. Pour the reaction solution into a 50 mL reaction kettle lined with polytetrafluoroethylene, keep it at 180 °C for 12 h. After the reaction kettle cools down, take out the reaction product, centrifuge at a speed of 15,000 revolutions per minute for 40 minutes. Then dissolve the precipitate in the DMF solution, and centrifuge again at a speed of 15,000 revolutions per minute for 20 minutes. Take the supernatant as the modified GQDs solution, and obtain the M-GQDs powder after removing the solvent by rotary evaporation.

[0100] 3) Select high-purity Al2O3, B2O3, SiO2, and ZnO as the raw materials for the glass matrix. The molar percentages of each raw material are: Al2O3 14%, B2O3 45%, SiO2 33%, ZnO 8%. Weigh the raw materials of Al2O3, B2O3, SiO2, and ZnO, and fully grind and mix them evenly in an agate mortar to obtain a glass matrix mixture. Place the glass matrix mixture in a corundum crucible, heat it to 1350 °C and keep it for 1 h. Then pour the glass melt into water for quenching to obtain precursor glass slag, and further crush it to obtain aluminoborosilicate-based glass-ceramic powder.

[0101] 4) Uniformly mix the aluminoborosilicate-based glass-ceramic powder with the graphene quantum dot material (the volume ratio of GQDs to M-GQDs is fixed at 1:1) to obtain a mixture. Transfer the mixture to a mold and form a green body by cold isostatic pressing (where the mass ratio of graphene quantum dots is 30 wt% of the precursor glass matrix). Then heat the green body in an air atmosphere to 680 °C and keep it for 1 h to obtain the optoelectronic glass.

[0102] Example 2

[0103] Provide an optoelectronic glass, which is prepared according to the following steps:

[0104] 1) Weigh 0.1 g of fullerene and 0.4 g of potassium peroxymonosulfate, add them to 20 mL of DMF, and ultrasonically disperse for 1.5 h to obtain a reaction solution. Pour the reaction solution into a 50 mL reaction kettle lined with polytetrafluoroethylene, keep it at 200 °C for 12 h. After the reaction kettle cools down, take out the reaction product, and then centrifuge the reaction product at a speed of 4,000 revolutions per minute for 40 minutes to remove the remaining potassium peroxymonosulfate and large residues. Take the supernatant and first filter it with a 0.22 μm filter membrane, and then dialyze it with a semipermeable membrane with a molecular weight cut-off of 3500 Da for three days to obtain the graphene quantum dot (GQDs) solution, and obtain the GQDs powder after removing the solvent by rotary evaporation.

[0105] 2) Weigh 5 mL of the GQDs aqueous solution and mix it with 10 mg of 2,3-diaminonaphthalene, add them to 20 mL of DMF, and ultrasonically disperse for 1.5 h to obtain a reaction solution. Pour the reaction solution into a 50 mL reaction kettle lined with polytetrafluoroethylene, keep it at 180 °C for 12 h. After the reaction kettle cools down, take out the reaction product, centrifuge at a speed of 15,000 revolutions per minute for 40 minutes, then dissolve the precipitate in the DMF solution, and centrifuge again at a speed of 15,000 revolutions per minute for 20 minutes. Take the supernatant as the modified GQDs solution, and obtain M-GQDs powder after removing the solvent by rotary evaporation.

[0106] 3) Select high-purity Al2O3, B2O3, SiO2, ZnO as the raw materials for the glass matrix. The molar percentages of each raw material are: Al2O3 14%, B2O3 45%, SiO2 39%, ZnO 2%. Weigh the raw materials of Al2O3, B2O3, SiO2, ZnO and grind and mix them evenly in an agate mortar to obtain a glass matrix mixture. Place the glass matrix mixture in a corundum crucible, heat it to 1350 °C and keep it for 1 h, then pour the glass melt into water for quenching to obtain precursor glass fragments, and further crush them to obtain aluminoborosilicate-based glass-ceramic powder.

[0107] 4) Uniformly mix the aluminoborosilicate-based glass-ceramic powder with the graphene quantum dot material (the volume ratio of GQDs to M-GQDs is fixed at 2:1) to obtain a mixture, transfer the mixture to a mold, and form a green body by cold isostatic pressing (where the mass ratio of graphene quantum dots is 30 wt% of the precursor glass matrix). Then heat the green body in an air atmosphere to 680 °C and keep it for 1 h to obtain the optoelectronic glass.

[0108] Experimental Example 1

[0109] Use a transmission electron microscope to detect the microstructure of the optoelectronic glass prepared in Example 1 and Example 2. The results are shown in the appendix Figure 1 .

[0110] From Figure 1 it can be clearly observed the presence of graphene quantum dots (black dots) and the glass phase (gray part). At the same time, it can be seen that a large number of graphene quantum dots are evenly distributed in the glass matrix without agglomeration, further confirming that the prepared optoelectronic glass has good transmittance performance, which helps to improve the luminous efficiency and luminous uniformity of high-power white light illumination devices.

[0111] Experimental Example 2

[0112] Detect the transmittance performance of the optoelectronic glass prepared in Example 1 and Example 2.

[0113] Detection method: The transmittance performance of the optoelectronic glass was tested using a UV-2600 ultraviolet-visible spectrophotometer produced by Shimadzu Corporation of Japan.

[0114] Test conditions: The scanning range was 200 nm to 1000 nm, the step size was 1 nm, the slit widths of the incident light and the outgoing light were both 5 nm, and the test was carried out at room temperature. The test results are shown in Figure 2 .

[0115] Figure 2 shows the transmittance spectra of the optoelectronic glasses prepared in Examples 1 and 2. From Figure 2 it can be seen that the transmittance of the optoelectronic glass is above 80%, indicating high optical performance.

[0116] Experimental Example 3

[0117] The luminescence properties of the optoelectronic glasses prepared in Example 1 and Example 2 were detected.

[0118] Detection method: The luminescence properties of the optoelectronic glass were tested using an FLS980 combined fluorescence spectrometer produced by Edinburgh Instruments of the UK. The optoelectronic glass was placed on a solid sample holder, and the excitation spectrum and the emission spectrum could be scanned respectively, with a wavelength range of 280 nm to 760 nm. In order to avoid the interference of the second harmonic peak of the incident light on the emission spectrum, corresponding filters could be added between the sample chamber and the emission light detection end.

[0119] Test conditions: The light source was a 450 W xenon lamp, the slit width of the monochromator could be adjusted according to the luminescence intensity, the step size was 1 nm, and the test was carried out at room temperature. The test results are shown in Figure 3 .

[0120] Figure 3 shows the PL spectrum and the CIE 1931 chromaticity coordinates of the optoelectronic glasses prepared in Example 1 and Example 2 under 385 nm laser irradiation.

[0121] From Figure 3 it can be seen that the PL spectrum of the optoelectronic glass covers a very wide range in the visible light region, that is, from the blue light (400 nm) to the red-orange light (700 nm) region, and white light emission can be achieved. Its CIE 1931 color coordinates (0.332, 0.336) are very close to the color coordinates of the standard white light (0.33, 0.33), indicating excellent luminescence properties.

[0122] Experimental Example 4

[0123] The thermal stability of the optoelectronic glasses prepared in Example 1 and Example 2 was detected.

[0124] Detection method: The FLS980 combined fluorescence spectrometer produced by Edinburgh Instruments in the UK was used to test the thermal stability of the optoelectronic glass. In high-power LD devices, the fluorescence conversion material receives a large amount of radiation from the high-energy density chip, resulting in its operating temperature being much higher than room temperature. Therefore, it is very necessary to detect the heat resistance of the sample. First, the prepared optoelectronic glass was heated from room temperature to 320 °C and then cooled to room temperature, and the luminescence intensity of the sample was measured after each heating-cooling cycle. The detection results are shown in Figure 4 。

[0125] Figure 4 The luminescence intensity diagrams of the optoelectronic glasses prepared in Example 1 and Example 2 after heating-cooling cycles in the range from room temperature to 320 °C are shown.

[0126] From Figure 4 It can be seen that after ten heating-cooling cycles, the luminescence intensity of the optoelectronic glass hardly changes, showing excellent thermal stability.

[0127] Experimental Example 5

[0128] The luminescence uniformity of the optoelectronic glasses prepared in Example 1 and Example 2 was detected.

[0129] Detection method: A hemispherical angular fixture was placed on the white light LD to measure the luminescence characteristics at different angles. The aperture was controlled at intervals of 10° to detect the luminescence intensity passing through a specific aperture. The detection results are shown in Figure 5 。

[0130] Figure 5 The angular distribution diagrams of the luminescence intensity of the laser illumination devices based on the optoelectronic glasses prepared in Example 1 and Example 2 are shown.

[0131] From Figure 5 It can be seen that the laser illumination devices based on the optoelectronic glasses prepared in the embodiments of the present application have good luminescence uniformity.

[0132] Experimental Example 6

[0133] The device stability of the optoelectronic glasses prepared in Example 1 and Example 2 was detected.

[0134] Detection method: The LABSPHEERE measurement system composed of an optical fiber spectrometer and an integrating sphere was used to test the stability performance of the white light LD device after working for different times under a high-power driving current. The detection results are shown in Figure 6 。 Figure 6 The emission intensities of the laser illumination devices of the optoelectronic glasses prepared in Example 1 and Example 2 at different working times (driving current is 1200 mA) are shown.

[0135] From Figure 6It can be seen that the luminous intensity of the laser lighting device of the optoelectronic glass still remains at 95% after continuous operation for 300 min, indicating good device stability.

[0136] The foregoing is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, various changes and modifications can be made to the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included within the protection scope of the present application.

Claims

1. An optoelectronic glass, characterized in that, Comprising: Light-emitting points and a matrix; The light-emitting points are dispersed in the matrix; The light-emitting points are graphene quantum dot materials, the matrix is an aluminoborosilicate glass-ceramic, and the aluminoborosilicate glass-ceramic is an Al2O3-B2O3-SiO2-ZnO system; By mass percentage, the mass of the light-emitting points is 20% - 40% of the matrix; The preparation method of the optoelectronic glass includes: After uniformly mixing the graphene quantum dot material and the aluminoborosilicate glass-ceramic powder, keep it at 650 °C - 750 °C for 0.5 h - 1.5 h.

2. The optoelectronic glass according to claim 1, wherein The graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots; among them, the carbon source of the graphene quantum dots is fullerene; The modified graphene quantum dots are the graphene quantum dots modified by 2,3-diaminonaphthalene.

3. The optoelectronic glass according to claim 2, wherein In the graphene quantum dot material, the volume ratio of the graphene quantum dots to the modified graphene quantum dots is 0.5:1 - 2:

1.

4. The optoelectronic glass according to claim 1, wherein The emission wavelength of the graphene quantum dot material is 400 nm - 700 nm.

5. The optoelectronic glass according to any one of claims 1 - 4, wherein The thickness of the optoelectronic glass is 1.35 mm - 2.35 mm.

6. The optoelectronic glass according to claim 1, wherein The aluminoborosilicate glass-ceramic includes: 5 mol% - 20 mol% alumina, 40 mol% - 60 mol% boric oxide, 25 mol% - 45 mol% silica, 0.1 mol% - 10 mol% zinc oxide.

7. The optoelectronic glass according to claim 1, wherein The preparation method of the optoelectronic glass includes: The graphene quantum dot material includes graphene quantum dots and modified graphene quantum dots; Preparing the graphene quantum dots includes: Reacting a mixture of fullerene and potassium peroxymonosulfate at 140 °C - 200 °C for 2 h - 14 h; then making the obtained reactant into a powder.

8. The optoelectronic glass according to claim 7, wherein, Preparing the modified graphene quantum dots includes: Mixing the graphene quantum dots and 2,3-diaminonaphthalene uniformly, then reacting at 170 °C - 190 °C for 12 h - 15 h, and making the reactant into a powder.

9. A light-emitting device, characterized in that, Comprising: The optoelectronic glass according to any one of claims 1 - 8.

Images