CN112993142B - Three-dimensional high-thermal-conductivity white light LED and preparation method thereof - Google Patents
Three-dimensional high-thermal-conductivity white light LED and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/64—Heat extraction or cooling elements
- H01L33/641—Heat extraction or cooling elements characterized by the materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/64—Heat extraction or cooling elements
- H01L33/642—Heat extraction or cooling elements characterized by the shape
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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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- Led Device Packages (AREA)
Abstract
The invention belongs to the field of white light LED packaging, and particularly discloses a three-dimensional high-thermal-conductivity white light LED and a preparation method thereof, wherein the three-dimensional high-thermal-conductivity white light LED comprises a substrate, a reflective cavity, an LED chip and a three-dimensional high-thermal-conductivity fluorescent colloid, wherein the reflective cavity is arranged on the substrate, the LED chip is positioned in the reflective cavity and fixed on the surface of the substrate, and the LED chip is connected with a lead component; the three-dimensional high-thermal-conductivity fluorescent colloid is filled in the reflecting cavity and covers the LED chip, and the three-dimensional high-thermal-conductivity fluorescent colloid consists of a three-dimensional high-thermal-conductivity framework and quantum dot colloids filled in gaps of the three-dimensional high-thermal-conductivity framework. The invention can enable light energy to smoothly emit from the three-dimensional high-heat-conductivity framework, ensures the luminous efficiency of the white light LED, reduces the working temperature of the fluorescent colloid, improves the long-term reliability of the fluorescent colloid, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of white light LED packaging, and particularly relates to a three-dimensional high-thermal-conductivity white light LED and a preparation method thereof.
Background
A white Light Emitting Diode (LED) is a semiconductor Light Emitting device based on the P-N junction electroluminescence principle. As a fourth generation illumination light source, the LED has the advantages of high electro-optic conversion efficiency, long service life, energy saving, environmental protection, compact structure, and the like, and is recognized as one of the high technical fields with the greatest development prospects in the 21 st century.
White LEDs are typically formed by encapsulating a blue LED chip with a phosphor material. The traditional fluorescent material is mainly yellow fluorescent powder, and a white light LED obtained by exciting the yellow fluorescent powder through a blue light chip has high luminous efficiency, but the white light LED has unsaturated color and low color rendering index due to lack of red light. As a new nano-scale light conversion material, the emission spectrum of the quantum dot can be regulated by changing the size and the components, and the emitted color has extremely high purity. Therefore, in current high quality white LEDs, yellow phosphor and red quantum dots are typically added to the encapsulant as the phosphor material.
In the white light LED, since the phosphor and the quantum dot generate energy loss during the light conversion process, the phosphor micro-particles and the quantum dot nano-particles are equivalent to thousands of micro/nano heating sources, which causes the temperature of the phosphor to rise, and the high temperature will reduce the light conversion efficiency of the phosphor, and finally threaten the light emitting efficiency and long-term reliability of the white light LED. Because the fluorescent powder and the quantum dots are dispersed in the polymer colloid with extremely low heat conductivity coefficient, the technical problem is difficult to solve by the conventional heat dissipation methods such as air cooling and liquid cooling.
Due to the above drawbacks and deficiencies, there is a need in the art to provide an effective method for reducing the operating temperature of the fluorescent material without affecting the light emitting performance of the white LED, so as to ensure the long-term reliability of the white LED.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides the three-dimensional high-thermal-conductivity white light LED and the preparation method thereof, the heat conductivity coefficient of the fluorescent colloid is effectively improved by constructing the three-dimensional high-thermal-conductivity framework, so that the heat productivity of the fluorescent powder and the quantum dots is rapidly LED out of the fluorescent colloid, and the aim of reducing the working temperature of the fluorescent colloid is further achieved.
In order to achieve the above object, according to one aspect of the present invention, a three-dimensional high thermal conductivity white LED is provided, which includes a substrate, a reflective cavity, an LED chip, and a three-dimensional high thermal conductivity fluorescent colloid, wherein:
the LED chip is positioned in the reflecting cavity and fixed on the surface of the substrate, and the LED chip is connected with a lead component;
the three-dimensional high-thermal-conductivity fluorescent colloid is filled in the reflective cavity and covers the LED chip, and the three-dimensional high-thermal-conductivity fluorescent colloid consists of a three-dimensional high-thermal-conductivity framework and quantum dot colloids filled in gaps of the three-dimensional high-thermal-conductivity framework.
Preferably, the lead part comprises a lead frame and a lead, the lead frame is arranged on the reflective cavity, one end of the lead is connected with the LED chip, and the other end of the lead is connected with the lead frame; preferably, the LED chip is a forward, flip or vertical structure with the substrate being sapphire, silicon or silicon carbide.
According to another aspect of the present invention, a method for preparing a three-dimensional white LED with high thermal conductivity is provided, which includes the following steps:
s1, assembling the substrate, the light reflecting cavity, the LED chip and the lead component together;
s2, mixing deionized water, alkyl glycoside, non-light-absorbing heat-conducting filler, fluorescent powder, curdlan and gellan gum according to a preset proportion, and then stirring and heating to obtain a volume-expanded mixed solution;
s3, injecting the mixed solution into the assembled reflection cavity, and cooling to obtain a three-dimensional high-heat-conductivity framework;
s4, preparing quantum dot colloid, injecting the quantum dot colloid into the three-dimensional high-thermal-conductivity framework, filling the quantum dot colloid in gaps of the three-dimensional high-thermal-conductivity framework, and curing to obtain the three-dimensional high-thermal-conductivity white light LED.
As a further preferred method, in step S2, the mixing ratio of the deionized water, the alkyl glycoside, the non-light-absorbing and heat-conducting filler, the phosphor, curdlan and gellan gum is: in each 100ml of deionized water, the addition amount of the alkyl glycoside is 0.5ml to 5ml, the addition amount of the non-light-absorbing heat-conducting filler is 2.5g to 15g, the addition amount of the fluorescent powder is 1g to 10g, the addition amount of the curdlan is 0.5g to 5g, and the addition amount of the gellan gum is 0.5g to 5 g.
As further preferred, the non-light-absorbing and heat-conducting filler is aluminum nitride, aluminum oxide, boron nitride, the average particle size is 5 μm to 50 μm, and the boron nitride is preferably hexagonal boron nitride; preferably, the fluorescent powder is YAG or TAG, the average particle size is 10-20 μm, and the light-emitting wavelength is 500-600 nm.
More preferably, in step S2, the volume expansion ratio of the mixed solution is 2 to 6 times; preferably, the materials are mixed according to a preset proportion and then are placed in a magnetic stirrer, the materials are stirred at a high speed of 800-1500 rpm for 10-60 minutes to be fully dissolved and mixed, bubbles are introduced during stirring to expand the volume of the mixed solution, then the mixed solution is placed in a water bath heating stirrer, the curdlan molecules and the gellan gum molecules form a cross-linking structure under the conditions that the heating temperature is 85-95 ℃ and the rotating speed is 500-1500 rpm, and the volume of the mixed solution is continuously expanded to obtain the required volume expanded mixed solution.
Preferably, in step S3, after the mixed solution is injected into the reflective cavity, the mixed solution is cooled to room temperature to form a solid gel in the reflective cavity, and then the solid gel is dried in a freeze dryer to remove moisture in the solid gel, so as to obtain a three-dimensional high thermal conductivity skeleton; preferably, the freeze-drying time is 10 hours to 24 hours; preferably, the volume of the mixed liquid injected into the reflective cavity is 50-100% of the total volume of the reflective cavity.
As a further preferred method, in step S4, the quantum dot colloid is prepared as follows: and mixing the quantum dot nano-particle solution and the packaging adhesive according to a preset proportion, uniformly stirring, and removing bubbles in vacuum to obtain the required quantum dot colloid.
As further preferred, the volume ratio of the quantum dot nanoparticle solution to the encapsulation glue is 1:100-1: 10; preferably, the mass concentration of the quantum dot nanoparticle solution is 5-50 mg/ml; preferably, the average particle size of the quantum dot nanoparticles in the quantum dot nanoparticle solution is 10nm-20nm, the light-emitting wavelength is 600nm-700nm, the quantum dot nanoparticles are of a core-shell structure, and preferably one or more of cadmium selenide, cadmium sulfoselenide, indium phosphide, copper indium sulfide or perovskite; preferably, the encapsulation adhesive is silica gel, epoxy resin or liquid glass.
More preferably, in step S4, the resin composition is cured by heating under vacuum at a temperature of 80 ℃ to 150 ℃ and a vacuum degree of 15Pa or less.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the three-dimensional high-thermal-conductivity white LED developed by the invention, the three-dimensional high-thermal-conductivity skeleton is constructed in the fluorescent colloid, so that heat generated by fluorescent powder and quantum dots can be quickly conducted out through the three-dimensional skeleton, the temperature of a fluorescent material is further reduced, and the long-term working reliability of the white LED is improved.
2. According to the invention, through the development of a formula (comprising the composition of materials and the proportion of the materials) and the matching of proper stirring, heating and cooling processes, the three-dimensional high-thermal-conductivity fluorescent skeleton with a porous foam structure can be prepared, and because the three-dimensional high-thermal-conductivity fluorescent skeleton prepared by the invention is of the porous foam structure, light energy emitted by an LED chip and fluorescent powder/quantum dots can be emitted outwards through quantum colloids in holes of the skeleton, and through the addition of a non-light-absorbing heat-conducting filler, the scattering of the fluorescent colloid can be effectively enhanced.
3. According to the invention, through the matching of the quantum dot nano-particle solution and the packaging adhesive, the mass concentration of the quantum dot nano-particle solution, and the size and structure of the quantum dot nano-particle solution, the quantum dot luminescence spectrum matched with the LED chip and the fluorescent powder luminescence spectrum can be obtained, so that the high color rendering index is obtained, the luminous efficiency is maximized, and the photo-induced heating loss is minimized.
4. The invention can prepare the white light LED with high luminous efficiency and obviously reduced working temperature by adopting simple steps, has the characteristics of simple operation, low cost and the like, and is suitable for large-scale production.
5. Compared with the traditional white light LED, the three-dimensional high-heat-conductivity white light LED prepared by the invention has remarkable effects in heat conduction and temperature reduction, and the working temperature is lower than that of the traditional white light LED by more than 34 ℃.
Drawings
Fig. 1 is a schematic structural diagram of a three-dimensional high thermal conductivity white light LED provided in an embodiment of the present invention;
FIG. 2 is a flowchart of a method for manufacturing a three-dimensional white LED with high thermal conductivity according to an embodiment of the present invention;
fig. 3a is a schematic diagram of a plurality of LED chips packaged in the same reflective cavity provided in embodiment 4;
FIG. 3b is a schematic view of multiple light-reflecting cavities packaged on the same substrate as provided in example 4;
fig. 4a is a schematic view of multiple LED chips disposed on a PCB substrate and encapsulated in the same reflective cavity in embodiment 5;
FIG. 4b is a schematic diagram of multiple light-reflecting cavities packaged on the same PCB substrate provided in embodiment 5;
FIG. 5 is a scanning electron microscope physical image of the three-dimensional high thermal conductivity boron nitride skeleton prepared by the method of the present invention, wherein (a) is a scanning image of a low power lens and (b) is a scanning image of a high power lens;
FIG. 6 is a comparison graph of the luminescence spectra and optical properties of the three-dimensional high thermal conductivity white LED of the present invention and the conventional white LED;
fig. 7 is a graph of the actual measurement result of the surface temperature field when the three-dimensional high thermal conductivity white LED of the present invention and the conventional white LED operate at the same driving current.
The same reference numbers will be used throughout the drawings to refer to the same or like elements or structures, wherein:
101-substrate, 102-LED chip, 103-lead, 104-reflective cavity, 105-lead frame, 106-three-dimensional high thermal conductivity fluorescent colloid, 107-three-dimensional high thermal conductivity boron nitride skeleton, 108-mixed liquid, 109-beaker, 110-magnetic stirrer, 111-magnetic stirrer, 112-water bath heating stirrer, 113-quantum dot colloid, and 114-copper column.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, an embodiment of the present invention provides a three-dimensional white LED with high thermal conductivity, which includes a substrate 101, a reflective cavity 104, an LED chip 102, and a three-dimensional fluorescent colloid 106 with high thermal conductivity, where the reflective cavity 104 is mounted on the substrate 101, the LED chip 102 is located inside the reflective cavity 104 and fixed on the surface of the substrate 101, and the LED chip 102 is connected to a lead component; the three-dimensional high thermal conductivity fluorescent colloid 106 is filled in the reflective cavity 104 and covers the LED chip 102, and the three-dimensional high thermal conductivity fluorescent colloid 106 is composed of a three-dimensional high thermal conductivity skeleton and quantum dot colloids filled in gaps of the three-dimensional high thermal conductivity skeleton.
Specifically, the LED chip 102 is a front-side, flip-chip, or vertical structure, and the substrate thereof is sapphire, silicon, or silicon carbide. The lead part includes a lead 103 and a lead frame 105, the lead frame 105 is mounted on the reflective cavity 104, the lead 103 is preferably a gold wire, one end of which is connected to the LED chip 102, and the other end of which is connected to the lead frame 105. Through the setting of lead frame, can realize the electricity and connect in various service environment, satisfy different user demands.
As shown in fig. 2, an embodiment of the present invention further provides a method for preparing the three-dimensional high thermal conductivity white light LED, which includes the following steps:
s1, firstly, assembling the substrate 101, the reflective cavity 104, the LED chip 102 and the lead component together according to the relative positions of the substrate, the reflective cavity, the LED chip and the lead component according to the integral structure of the three-dimensional high-thermal-conductivity white light LED;
s2, mixing deionized water, alkyl glycoside, non-light-absorbing heat-conducting filler, fluorescent powder, curdlan and gellan gum according to a preset proportion, stirring and heating to obtain a volume-expanded mixed solution;
s3, injecting the volume expanded mixed solution into the assembled light reflecting cavity 104, cooling to obtain a three-dimensional high heat conduction framework, wherein the main body of the framework is non-light-absorbing heat conduction filler and fluorescent powder particles which are linked together by curdlan and gellan gum molecules to form a three-dimensional continuous high heat conduction channel, and the framework is internally provided with three-dimensionally communicated holes with the size of 100-500 mu m;
s4, finally, preparing quantum dot colloid, injecting the quantum dot colloid into the three-dimensional high-thermal-conductivity framework, filling the quantum dot colloid in gaps of the three-dimensional high-thermal-conductivity framework, and curing to obtain the three-dimensional high-thermal-conductivity white light LED. Generally, when the colloid on the surface of the three-dimensional high-thermal-conductivity framework does not penetrate into the framework, the colloid is considered to fill the framework gap.
In order to prepare the required three-dimensional high-thermal-conductivity framework, the preparation (type and proportion of materials) of the materials is crucial, the final type and proportion of the materials of the three-dimensional high-thermal-conductivity framework are determined by continuous exploration, namely deionized water, alkyl glycoside, non-light-absorbing heat-conducting filler, fluorescent powder, curdlan and gellan gum are taken as the materials and are prepared according to the following proportion: 0.5ml to 5ml of alkyl glycoside, 2.5g to 15g of non-light-absorbing heat-conducting filler, 1g to 10g of fluorescent powder, 0.5g to 5g of curdlan and 0.5g to 5g of gellan gum are added into each 100ml of deionized water. Under the above proportion, the viscosity of the mixed liquid is moderate, which is beneficial to stirring operation, and the proper amount of bubbles generated in the stirring process can extrude the heat-conducting filler into a continuous heat-conducting channel, which is beneficial to the generation of the subsequent three-dimensional heat-conducting framework, and the proper amount of the curdlan and the gellan gum is added, so that the three-dimensional heat-conducting framework has enough mechanical strength, which is beneficial to the perfusion of the subsequent colloid.
Wherein, deionized water is used as a solvent; the alkyl glycoside is used as a foaming agent, has the function of generating a large amount of bubbles in the stirring process of the mixed solution, and further generates a porous foam structure, and the adding amount of the alkyl glycoside determines the volume expansion degree of the mixed solution after stirring; the invention determines the optimal addition amount through continuous research, namely 2.5-15 g of non-light-absorbing heat-conducting filler is added into every 100ml of deionized water, so that the light emitting and heat conducting performance of an LED can be optimized under the addition amount. The curdlan and the gellan gum are both used as gelling agents and have the function of converting the mixed solution from jelly to solid through self gelling reaction in the process of heating and cooling the mixed solution. The two materials are selected because the polymer chain of the curdlan can crosslink the heat-conducting filler and the fluorescent powder together to form a three-dimensional structure, but researches find that the three-dimensional structure gel prepared from the curdlan has weak mechanical strength and is easy to collapse, so the invention further explores to solve the problem, finds that the solid mechanical strength of the three-dimensional structure after solidification can be improved after the gellan gum is added, and can effectively make up for the defect of collapse of the curdlan, but further researches find that the addition of the gellan gum is too much, which can cause the viscosity of the mixed solution to be increased and the fluidity to be poor, and causes difficulty in the preparation process of the three-dimensional framework, and therefore, deep researches need to be carried out on the addition amounts of the curdlan and the gellan gum. According to the invention, through continuous exploration and adjustment, the curdlan and the gellan gum are finally determined to be used as the gel for preparing the three-dimensional high-thermal-conductivity framework together, and the addition amount of the curdlan in each 100ml of deionized water is 0.5-5 g, and the addition amount of the gellan gum is 0.5-5 g, so that the smooth preparation of the three-dimensional framework structure can be ensured, and the strength meets the requirement.
More specifically, the non-light-absorbing and heat-conducting filler is aluminum oxide, aluminum nitride or boron nitride, the average particle size is 5-50 μm, and the boron nitride is hexagonal boron nitride preferably. Further, the fluorescent powder is YAG (cesium-doped yttrium aluminum garnet crystal fluorescent powder) or TAG (cerium-doped terbium aluminum garnet crystal fluorescent powder), the average particle size is 10-20 μm, and the light-emitting wavelength is 500-600 nm. The non-light-absorption heat-conducting filler has the advantages of high heat conductivity coefficient and low absorption effect on light energy, is beneficial to light emergence, can facilitate effective forming of a three-dimensional heat-conducting framework through the design of the particle size of the filler, can avoid particle precipitation, and further improves the uniformity of the framework holes. Through the design of the particle size of the fluorescent powder, the light absorption capacity can be ensured, so that blue light can be effectively converted into yellow light, and the precipitation can be avoided, so that the uniformity of light emission is guaranteed.
Further, in step S2, the volume expansion factor of the mixed liquid is 2-6 times, and the volume expansion of the mixed liquid indicates that bubbles have been generated in the mixed liquid, and the bubbles will form three-dimensionally interconnected pores after the mixed liquid is solidified and freeze-dried, thereby facilitating the emission of light energy. The porosity of the three-dimensional framework is determined by the expansion multiple of the volume, the too small porosity is not beneficial to light energy emergence, the too large porosity is not beneficial to forming a continuous heat conduction channel, and the light emitting performance and the heat conduction performance of the finally prepared LED can be ensured through the design of the expansion multiple. Preferably, the materials are mixed according to a preset proportion and then are placed in a magnetic stirrer, the materials are stirred at a high speed of 800-1500 rpm for 10-60 minutes to be fully dissolved and mixed, bubbles such as air bubbles are introduced during stirring to expand the volume of the mixed solution, then the mixed solution is placed in a water bath heating stirrer, the curdlan molecules and the gellan gum molecules form a cross-linking structure under the conditions that the heating temperature is 85-95 ℃ and the rotating speed is 500-1500 rpm, and the volume of the mixed solution is continuously expanded to obtain the mixed solution with the required volume expansion. When heating, curdlan and gellan gum are dispersed in water, the macromolecular chains of curdlan and gellan gum are crosslinked with each other, curdlan molecules can be crosslinked, gellan gum molecules can be crosslinked, curdlan molecules and gellan gum molecules can also be crosslinked, so that the heat-conducting filler and the fluorescent powder are confined in space, and a three-dimensional interconnected structure is formed. Under the process, all components in the mixed liquid are uniformly distributed in space, meanwhile, the non-light-absorbing heat-conducting filler forms a three-dimensionally interconnected high-heat-conducting framework under the crosslinking action of the high molecules and the extrusion action of the bubbles, a key heat-conducting effect is achieved in the subsequent process, three-dimensionally interconnected holes are formed in the space occupied by the bubbles after the freeze drying in the step S3, and a key light-emitting effect is achieved in the subsequent process.
Further, in step S3, after the mixed solution is injected into the reflective cavity, the mixed solution is cooled to room temperature to form a solid gel in the reflective cavity, and then the solid gel is dried in a freeze dryer to remove moisture in the solid gel, so as to obtain the three-dimensional high thermal conductivity skeleton. Through the process, moisture in the solid gel is extracted, and in the obtained three-dimensional high-thermal-conductivity framework, the non-light-absorption thermal-conductivity filler plays a key three-dimensional thermal-conductivity role, and the holes play a key light-emitting role. Preferably, the freeze-drying time is 10 hours to 24 hours, the moisture of the solid gel can be completely extracted under the process, meanwhile, the time of the preparation process is not too long, and the preparation efficiency is ensured. Preferably, the volume of the mixed liquid injected into the light reflecting cavity is 50% -100% of the total volume of the light reflecting cavity, and under the process, part of blue light emitted by the LED chip can be converted into yellow light and red light, so that a reasonable three-color spectrum is obtained.
Specifically, in step S4, the quantum dot colloid is prepared as follows: and mixing the quantum dot nano-particle solution and the packaging adhesive according to a preset proportion, uniformly stirring, and removing bubbles in vacuum to obtain the required quantum dot colloid. Specifically, the volume ratio of the quantum dot nanoparticle solution to the packaging adhesive is 1:100-1:10, and the quantum dot nanoparticles can be uniformly distributed in the system under the ratio, so that quantum dot colloid with uniform luminescence is obtained. Preferably, the mass concentration of the quantum dot nanoparticle solution is 5mg-50mg/ml, the average particle size of the quantum dot nanoparticles in the quantum dot nanoparticle solution is 10nm-20nm, the light-emitting wavelength is 600nm-700nm, the quantum dot nanoparticles are of a core-shell structure, and preferably one or more of cadmium selenide, cadmium sulfoselenide, indium phosphide, copper indium sulfide or perovskite. Under the concentration, the size and the structure, the quantum dot nano particles are not easy to precipitate and agglomerate in a system, stable luminescence is facilitated, and meanwhile, the luminescence spectrum of the quantum dot can be matched with the luminescence spectrum of a blue light LED chip and yellow fluorescent powder, so that a high-quality white light spectrum with high color rendering index is synthesized. The packaging adhesive is silica gel, epoxy resin or liquid glass.
More specifically, in step S4, heating and curing are performed under vacuum at 80-150 ℃ and under a vacuum degree of 15Pa, so as to obtain a compact solid luminescent colloid with moderate hardness, and to ensure that the luminescent efficiency of the phosphor and the quantum dots is not attenuated due to too high temperature during curing.
According to the invention, through the mutual matching of the process parameters such as the fluorescent powder, the quantum dots, the specific material of the three-dimensional high-thermal-conductivity framework, the size and the like, the luminous efficiency of the LED can be effectively improved, an ideal luminous spectrum can be obtained, the use requirements of different environments can be met, and meanwhile, the working temperature can be effectively reduced.
To better explain the invention, several specific examples are given below:
example 1
Referring to fig. 2, this example uses hexagonal boron nitride with an average particle size of 45 μm; the fluorescent powder is YAG, the average grain diameter is 13 μm, and the light-emitting wavelength is 538 nm; the packaging adhesive is silica gel; the average particle size of the quantum dot nano particles is 13nm, the light-emitting wavelength is 626nm, the chemical component is cadmium selenide, the mass concentration of a quantum dot nano particle solution is 10mg/ml, the LED chip is of a forward mounting structure, and the substrate is sapphire. The method specifically comprises the following steps:
s1, taking 100ml of deionized water, adding 1ml of alkyl glycoside (APG), 3g of boron nitride, 2.5g of fluorescent powder, 1g of curdlan and 1g of gellan gum to obtain a mixed solution 108, putting the mixed solution 108 on a magnetic stirrer 111, setting the rotating speed to 900 revolutions per minute, stirring for 15 minutes, fully dissolving the curdlan by high-speed stirring, and introducing a large amount of bubbles into the mixed solution 108 to expand the volume of the mixed solution 108;
s2, placing the mixed solution 108 in a water-bath heating stirrer 112, setting the heating temperature to 90 ℃ and the rotation speed to 600 revolutions per minute, heating to enable molecules of curdlan and gellan gum to form a cross-linked structure, and continuously expanding the volume of the mixed solution 108 to 3 times of the volume of the mixed solution before stirring in the step S1;
s3, sucking the mixed liquid 108 from the water-bath heating stirrer 112, quickly injecting the mixed liquid into the light-reflecting cavity 104 with the LED chip 102 in advance, wherein the volume of the mixed liquid injected into the light-reflecting cavity is 75% of the total volume of the light-reflecting cavity, placing the light-reflecting cavity at normal temperature to cool the mixed liquid 108 to room temperature, and forming solid gel in the light-reflecting cavity 104;
s4, drying the LED obtained in the step S3 in a freeze dryer for 12 hours, removing water in the solid gel, and obtaining an LED sample with a three-dimensional high-heat-conductivity boron nitride framework 107;
s5, mixing the quantum dot nano-particle solution and the packaging adhesive uniformly according to the volume ratio of 1:20, stirring uniformly, removing bubbles in vacuum to form a quantum dot colloid 113, injecting the quantum dot colloid 113 into the LED light reflecting cavity 104 obtained in the step S4, filling the quantum dot colloid 113 in the gap of the three-dimensional high-thermal-conductivity boron nitride framework 107 through multiple times of vacuumizing, and then heating and curing in vacuum at the temperature of 95 ℃ to obtain the three-dimensional high-thermal-conductivity white light LED.
Example 2
The present example used hexagonal boron nitride with an average particle size of 15 μm; the fluorescent powder is YAG, the average grain diameter is 18 μm, and the luminous wavelength is 558 nm; the packaging adhesive is silica gel; the average particle size of the quantum dot nano particles is 15nm, the light-emitting wavelength is 635nm, the chemical components are perovskite, the mass concentration of a quantum dot nano particle solution is 15mg/ml, the LED chip is a horizontal electrode chip, and the substrate is silicon. The method specifically comprises the following steps:
s1, taking 100ml of deionized water, adding 0.5ml of alkyl glycoside (APG), 2.5g of boron nitride, 1.5g of fluorescent powder, 0.5g of curdlan and 0.5g of gellan gum to obtain a mixed solution 108, putting the mixed solution 108 on a magnetic stirrer 111, setting the rotating speed to 1200 revolutions per minute, stirring for 10 minutes, fully dissolving the curdlan through high-speed stirring, and introducing a large amount of bubbles into the mixed solution 108 to expand the volume of the mixed solution 108;
s2, placing the mixed solution 108 in a water-bath heating stirrer 112, setting the heating temperature to 85 ℃ and the rotation speed to 900 revolutions per minute, heating to enable curdlan molecules and gellan gum molecules to form a cross-linked structure, and continuously expanding the volume of the mixed solution 108 to 2 times of the volume before stirring in the step S1;
s3, sucking the mixed liquid 108 from the water-bath heating stirrer 112, quickly injecting the mixed liquid into the light-reflecting cavity 104 with the LED chip 102 in advance, wherein the volume of the mixed liquid injected into the light-reflecting cavity is 50% of the total volume of the light-reflecting cavity, placing the light-reflecting cavity at normal temperature to cool the mixed liquid 108 to room temperature, and forming solid gel in the light-reflecting cavity 104;
s4, drying the LED obtained in the step S3 in a freeze dryer for 10 hours, removing water in the solid gel, and obtaining an LED sample with a three-dimensional high-heat-conductivity boron nitride skeleton 107;
s5, mixing the quantum dot nano-particle solution and the packaging adhesive uniformly according to the volume ratio of 1:100, stirring uniformly, removing bubbles in vacuum to form a quantum dot colloid 113, injecting the quantum dot colloid 113 into the LED light reflecting cavity 104 obtained in the step S4, filling the quantum dot colloid 113 in the gap of the three-dimensional high-thermal-conductivity boron nitride framework 107 through multiple times of vacuumizing, and then heating and curing in vacuum at the temperature of 85 ℃ to obtain the three-dimensional high-thermal-conductivity white light LED.
Example 3
In the embodiment, the non-light-absorption heat-conduction filler is aluminum nitride, and the average particle size is 5 μm; the fluorescent powder is TAG, the average particle size is 10 mu m, and the light-emitting wavelength is 520 nm; the packaging adhesive is silica gel; the average particle size of the quantum dot nanoparticles is 10nm, the light-emitting wavelength is 610nm, the chemical component is indium phosphide, the mass concentration of a quantum dot nanoparticle solution is 5mg/ml, the LED chip is a horizontal electrode chip, and the substrate is silicon. The method specifically comprises the following steps:
s1, taking 100ml of deionized water, adding 3ml of alkyl glycoside (APG), 5g of aluminum nitride, 1g of fluorescent powder, 2.5g of curdlan and 2g of gellan gum to obtain a mixed solution 108, putting the mixed solution 108 on a magnetic stirrer 111, setting the rotating speed to be 800 revolutions per minute, stirring for 30 minutes, fully dissolving the curdlan by high-speed stirring, and introducing a large amount of bubbles into the mixed solution 108 to expand the volume of the mixed solution 108;
s2, placing the mixed solution 108 in a water-bath heating stirrer 112, setting the heating temperature to 95 ℃ and the rotation speed to 1200 revolutions per minute, heating to enable curdlan molecules and gellan gum molecules to form a cross-linked structure, and continuously expanding the volume of the mixed solution 108 to 2.5 times of the volume before stirring in the step S1;
s3, sucking the mixed liquid 108 from the water-bath heating stirrer 112, quickly injecting the mixed liquid into the light-reflecting cavity 104 with the LED chip 102 in advance, wherein the volume of the mixed liquid injected into the light-reflecting cavity is 90% of the total volume of the light-reflecting cavity, placing the light-reflecting cavity at normal temperature to cool the mixed liquid 108 to room temperature, and forming solid gel in the light-reflecting cavity 104;
s4, drying the LED obtained in the step S3 in a freeze dryer for 20 hours, and removing water in the solid gel to obtain an LED sample with a three-dimensional high-heat-conductivity aluminum nitride framework 107;
s5, mixing the quantum dot nano-particle solution and the packaging adhesive uniformly according to the volume ratio of 1:50, stirring uniformly, removing bubbles in vacuum to form a quantum dot colloid 113, injecting the quantum dot colloid 113 into the LED light reflecting cavity 104 obtained in the step S4, filling the quantum dot colloid 113 in the gap of the three-dimensional high-thermal-conductivity aluminum nitride framework 107 through multiple times of vacuumizing, and then heating and curing in vacuum at the temperature of 130 ℃ to obtain the three-dimensional high-thermal-conductivity white light LED.
Example 4
Referring to fig. 3a and 3b, the present embodiment relates to an array type silicon-based package of multiple LED chips. The difference from embodiment 2 is that the LED chip 102 is a flip chip structure, the substrate is silicon, and multiple LED chips are packaged in the same reflective cavity, as shown in fig. 3a, or multiple reflective cavities are packaged on the same substrate, as shown in fig. 3 b.
Example 5
Referring to fig. 4a and 4b, the present embodiment relates to an LED Printed Circuit Board (PCB) package. The difference from embodiment 4 is that the PCB substrate has a through hole structure, the through hole is filled with a copper pillar 114 with high thermal conductivity or other metal structures, and the LED chip is fixed on the copper pillar filled in the printed circuit board. As shown in fig. 4a, a plurality of LED chips are packaged in the same reflective cavity, and as shown in fig. 4b, a plurality of reflective cavities are packaged on the same PCB substrate.
Fig. 5 is a scanning electron microscope physical image of a three-dimensional high thermal conductivity framework prepared by the method of the present invention, wherein (a) is a scanned image under a low power mirror, and (b) is a scanned image under a high power mirror, and it can be seen from the images that the three-dimensional high thermal conductivity framework prepared by the present invention contains two key structures, one of which is a continuous three-dimensional framework structure (three-dimensionally interconnected high thermal conductivity network) as a thermal conductivity channel, which is beneficial to rapid heat conduction; the other is a three-dimensional communicated hole structure, which is beneficial to smooth emergence of light energy.
Fig. 6 is a comparison graph of the light emission spectrum and the optical performance of the three-dimensional high thermal conductivity white LED prepared by the method of the present invention and the white LED prepared by the conventional method, and it can be seen through comparison that the white LED having the three-dimensional thermal conductivity skeleton can obtain the same light emission spectrum and light emission efficiency as the conventional white LED, which indicates that the introduction of the three-dimensional thermal conductivity skeleton does not cause the change of the light emission performance of the white LED, and at the same time, the thermal conductivity can be significantly enhanced.
Fig. 7 is a graph of measured surface temperature field results for two types of white LEDs operating at the same drive current. The comparison of the two shows that the three-dimensional high-thermal-conductivity white light LED prepared by the invention can greatly reduce the working temperature of the fluorescent colloid under the same color temperature and luminous efficiency, and is 34.7 ℃ lower than that of the traditional white light LED, so that the high-thermal-conductivity white light LED has remarkable effects in heat conduction and cooling.
According to the three-dimensional high-thermal-conductivity white light LED provided by the invention, the thermal conductivity of the colloid is greatly improved through the three-dimensional interconnected high-thermal-conductivity network, so that the heat generated by the fluorescent material is rapidly LED out, and the beneficial effect of reducing the working temperature of the white light LED is realized.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (16)
1. The preparation method of the three-dimensional high-thermal-conductivity white light LED is characterized in that the three-dimensional high-thermal-conductivity white light LED comprises a substrate (101), a reflecting cavity (104), an LED chip (102) and a three-dimensional high-thermal-conductivity fluorescent colloid (106), wherein the reflecting cavity (104) is installed on the substrate (101), the LED chip (102) is located in the reflecting cavity (104) and fixed on the surface of the substrate (101), and the LED chip (102) is connected with a lead component; the three-dimensional high-thermal-conductivity fluorescent colloid (106) is filled in the light reflecting cavity (104) and covers the LED chip (102), and the three-dimensional high-thermal-conductivity fluorescent colloid (106) consists of a three-dimensional high-thermal-conductivity framework and quantum dot colloids filled in gaps of the three-dimensional high-thermal-conductivity framework; the preparation method comprises the following steps:
s1, assembling the substrate (101), the light reflecting cavity (104), the LED chip (102) and the lead component together;
s2, mixing deionized water, alkyl glycoside, non-light-absorbing heat-conducting filler, fluorescent powder, curdlan and gellan gum according to a preset proportion, and then stirring and heating to obtain a volume-expanded mixed solution;
s3, injecting the mixed solution into the assembled reflecting cavity (104), and cooling to obtain a three-dimensional high-thermal-conductivity framework;
s4, preparing quantum dot colloid, injecting the quantum dot colloid into the three-dimensional high-thermal-conductivity framework, filling the quantum dot colloid in gaps of the three-dimensional high-thermal-conductivity framework, and curing to obtain the three-dimensional high-thermal-conductivity white light LED.
2. The method according to claim 1, wherein in step S2, the deionized water, the alkyl glycoside, the non-light-absorbing and heat-conducting filler, the phosphor, the curdlan and the gellan gum are mixed in a ratio of: in each 100ml of deionized water, the addition amount of the alkyl glycoside is 0.5ml to 5ml, the addition amount of the non-light-absorbing heat-conducting filler is 2.5g to 15g, the addition amount of the fluorescent powder is 1g to 10g, the addition amount of the curdlan is 0.5g to 5g, and the addition amount of the gellan gum is 0.5g to 5 g.
3. The preparation method according to claim 1, characterized in that the non-light-absorbing, heat-conducting filler is aluminum nitride, aluminum oxide or boron nitride, and the average particle size is 5 μm to 50 μm.
4. The method of claim 3, wherein the boron nitride is hexagonal boron nitride.
5. The preparation method according to claim 1, wherein the phosphor is YAG or TAG, the average particle size is 10 μm to 20 μm, and the emission wavelength is 500nm to 600 nm.
6. The method according to claim 1, wherein in step S2, the volume expansion ratio of the mixed solution is 2 to 6 times.
7. The preparation method of claim 1, wherein the materials are mixed according to a preset ratio, then placed in a magnetic stirrer, stirred at a high speed of 800-1500 rpm for 10-60 minutes to fully dissolve and mix the materials, bubbles are introduced during stirring to expand the volume of the mixed solution, then the mixed solution is placed in a water bath heating stirrer, under the conditions that the heating temperature is 85-95 ℃ and the rotating speed is 500-1500 rpm, the curdlan molecules and the gellan gum molecules form a cross-linked structure, and the volume of the mixed solution is continuously expanded to obtain the mixed solution with the required volume expansion.
8. The method of claim 1, wherein in step S3, after the mixed liquid is injected into the reflective cavity, the mixed liquid is cooled to room temperature to form a solid gel in the reflective cavity, and then the solid gel is dried in a freeze dryer to remove water from the solid gel, thereby obtaining the three-dimensional high thermal conductivity skeleton.
9. The method of claim 8, wherein the freeze-drying time is from 10 hours to 24 hours.
10. The method of claim 8, wherein the volume of the mixture injected into the reflective cavity is 50% to 100% of the total volume of the reflective cavity.
11. The method of claim 1, wherein in step S4, the quantum dot colloid is prepared by: and mixing the quantum dot nano-particle solution and the packaging adhesive according to a preset proportion, uniformly stirring, and removing bubbles in vacuum to obtain the required quantum dot colloid.
12. The preparation method of claim 11, wherein the volume ratio of the quantum dot nanoparticle solution to the encapsulation glue is 1:100 to 1: 10.
13. The method of claim 11, wherein the quantum dot nanoparticle solution has a mass concentration of 5 to 50 mg/ml; the average particle size of the quantum dot nanoparticles in the quantum dot nanoparticle solution is 10nm-20nm, the light-emitting wavelength is 600nm-700nm, and the quantum dot nanoparticles are of a core-shell structure.
14. The method of claim 13, wherein the quantum dot nanoparticles are one or more of cadmium selenide, cadmium sulfoselenide, indium phosphide, copper indium sulfide, or perovskite.
15. The method of claim 11, wherein the encapsulant is silicone, epoxy, or liquid glass.
16. The production method according to any one of claims 1 to 15, wherein in step S4, the heating and curing are performed under vacuum at a temperature of 80 ℃ to 150 ℃ and a vacuum degree of 15Pa or less.
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