A self-repairing aluminosilicate inorganic adhesive and deep ultraviolet LED all-inorganic packaging method

By using self-healing aluminosilicate inorganic adhesive composed of diamond powder, sodium silicate solution and fly ash, the problems of defects such as pores and cracks during the curing process of inorganic adhesive are solved, and the self-repair of inorganic adhesive curing is achieved, which significantly improves the airtightness and reliability of deep ultraviolet LED packaging.

CN117925115BActive Publication Date: 2025-05-06CHUANYING SEMICONDUCTOR TECHNOLOGY (SUZHOU) CO LTD
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Patent Information

Application Number
CN202410111296.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-25
Publication Date
2025-05-06
Estimated Expiration
2044-01-25

AI Technical Summary

Technical Problem

The existing aluminosilicate inorganic adhesives are prone to micro defects such as pores and cracks during the curing process, resulting in poor airtightness of deep ultraviolet LED packaging, affecting service life and reliability.

Method used

Self-healing aluminosilicate inorganic adhesive composed of diamond powder, sodium silicate solution and fly ash is used to promote the generation of mineral crystal phases and the flow of inorganic adhesives through the thermal storage and rapid thermal conduction of diamond powder, fill pores and cracks, and realize self-healing of the solidified body.

Benefits of technology

It significantly improves the density of the aluminosilicate inorganic adhesive cured body, reduces porosity and micro defects, enhances compressive strength and shear strength with the matrix material, improves the airtightness of deep ultraviolet LED packaging, and extends service life and reliability.

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Abstract

The present application provides a self-repairing aluminosilicate inorganic glue and a method for fully inorganic packaging of deep ultraviolet LEDs, belonging to the field of electronic packaging technology. The self-repairing aluminosilicate inorganic glue comprises the following components: 0-8wt% diamond powder; 41-45wt% sodium silicate solution; 51-56wt% fly ash. The self-repairing aluminosilicate inorganic glue of the present application can realize the self-repair of the defect problem of the inorganic glue solid body, enhance the self-healing performance of the inorganic glue solid body at room temperature or slightly above room temperature, have fewer defects at room temperature or slightly above room temperature, effectively improve the shear strength between the aluminosilicate inorganic glue and the matrix material and the packaging airtightness of the deep ultraviolet LED, and the self-repairing behavior of the aluminosilicate inorganic glue can significantly improve the service life and reliability of the deep ultraviolet LED.
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Description

Technical Field

[0001] The present application belongs to the field of electronic packaging technology, and more specifically, relates to a self-repairing aluminosilicate inorganic adhesive and a deep ultraviolet LED all-inorganic packaging method. Background Art

[0002] Deep ultraviolet LED packaging technology mainly includes transistor shape packaging technology, semi-inorganic packaging technology and full inorganic packaging technology. Although the transistor shape packaging technology has high reliability and good airtightness, the structure contains metal pins, resulting in a large structural size, which is not conducive to chip heat dissipation. Semi-inorganic packaging is to mount the deep ultraviolet LED chip in the ceramic substrate dam, and then use organic glue such as epoxy resin or silicone to fix the quartz glass cover on the ceramic substrate dam. However, due to the short wavelength and high energy of deep ultraviolet light, the organic glue will undergo ultraviolet degradation under long-term deep ultraviolet light radiation. The high thermal stress and temperature load in the module will also cause the organic glue to have defects such as yellowing, aging, and carbonization, which seriously affects the airtightness and service life of the deep ultraviolet LED package. Deep ultraviolet LEDs must be fully inorganically packaged using inorganic materials.

[0003] Aluminosilicate inorganic glue can form a three-dimensional network structure polymer solid body composed of structural units such as silicon oxygen and aluminum oxygen tetrahedron through alkali excitation reaction. The carbon emissions in the reaction process are greatly reduced compared with Portland cement. It is a green and low-carbon material with the advantages of resistance to ultraviolet radiation, low temperature curing, fast setting and early strength, good adhesion, heat resistance and acid and alkali corrosion resistance. Compared with organic glue, the use of aluminosilicate inorganic glue to encapsulate deep ultraviolet LEDs has obvious advantages.

[0004] Aluminosilicate inorganic glue is a polyaluminosilicate gelling material with a spatial network structure composed of [SiO4] and [AlO4] tetrahedral structural units alternately bonded by shared oxygen. During the polycondensation reaction, the dehydration process is accompanied by the self-shrinkage of the gelling material, which leads to a large number of defects such as pores and cracks in the inorganic glue solid body, making it impossible to achieve airtight packaging of deep ultraviolet LEDs, which seriously affects the service life and reliability of deep ultraviolet LEDs.

[0005] In order to reduce micro defects such as pores and cracks in the inorganic glue solid body and improve the density of the inorganic glue solid body, in the existing technology, domestic and foreign researchers have used nutrients, microorganisms, bacteria and spores to achieve self-repair of aluminosilicate inorganic glue. However, it is difficult for the above-mentioned active substances to survive and maintain stability in the high temperature and high humidity environment when the deep ultraviolet LED is working, and the above-mentioned substances are also difficult to withstand the high-intensity extrusion during mechanical stirring of the raw materials. Summary of the invention

[0006] Based on the chemical stability and efficient thermal conductivity of diamond, the purpose of this application is to provide a self-repairing aluminosilicate inorganic glue and a deep ultraviolet LED all-inorganic packaging method, thereby improving the airtightness of the deep ultraviolet LED packaging.

[0007] To achieve the above objectives, the first aspect of the present application provides a self-repairing aluminosilicate inorganic adhesive, comprising the following components:

[0008] Diamond powder 0~8wt%;

[0009] Sodium silicate solution 41-45wt%;

[0010] Fly ash 51~56wt%.

[0011] Furthermore, the particle size of the diamond powder is 2-4 μm, and the impurity content is less than 0.05 wt%. For example, the particle size of the diamond powder can be 2.5 μm, 3.5 μm, etc. The diamond powder mainly plays a role in heat storage and rapid heat conduction, thereby promoting the formation of mineral crystal phases and the flow of inorganic glue. Diamond powder with a smaller particle size can ensure that it will not affect the dissolution-depolymerization-condensation reaction between the aluminosilicate inorganic glue precursor and the alkali activator due to its own large volume while ensuring the above advantages.

[0012] Furthermore, the content of the diamond powder is 2.5-5.5wt%, for example, 2.7wt%, 5.26wt%, etc. Too high a content of diamond powder will hinder the alkali-induced reaction, causing incomplete dissolution-depolymerization-condensation reaction of some inorganic glue components, thereby significantly increasing the fluidity of the inorganic glue, while its own compressive strength and its shear strength with the matrix material will decrease; the porosity will increase, making the airtightness of the deep ultraviolet LED package worse.

[0013] Furthermore, the fly ash is composed of large-size particles and small-size particles, the particle size of the large-size particles is 55-60um, the particle size of the small-size particles is 1-2um, and the weight ratio of the small-size particles to the large-size particles is 1:3-5. For example, the particle size of the large-size particles is 57.65um, and the particle size of the small-size particles is 1.62um. In the fly ash of the present application, SiO2 accounts for 57.20wt%, Al2O3 accounts for 23.40wt%, Fe2O3 accounts for 6.20wt%, CaO accounts for 5.70wt%, MgO accounts for 2.10wt%, K2O accounts for 2.50wt%, SO3 accounts for 2.1wt%, and the loss on ignition accounts for 0.5wt%. The large-particle fly ash plays the main role in the condensation reaction with the alkaline activator, which will significantly affect the performance of the inorganic glue; the small-particle fly ash plays the role of filling the large-particle fly ash, which can make the fly ash reach a certain stacking density and promote the density of the aluminosilicate inorganic glue solidification body and the airtightness of the deep ultraviolet LED packaging.

[0014] Furthermore, the weight ratio of the small-size particles to the large-size particles is 1:4.

[0015] Furthermore, the concentration of the sodium silicate solution is 39-41° Bé. For example, it can be 40° Bé, consisting of 23.83wt% SiO2, 10.25wt% Na2O, and the rest is water. Controlling the concentration of the sodium silicate solution can ensure that the aluminosilicate inorganic glue will not affect the subsequent screen printing molding quality and the performance of the inorganic glue cured body due to its concentration being too thick or too thin.

[0016] The second aspect of the present application provides an application of a self-repairing aluminosilicate inorganic adhesive in LED packaging.

[0017] The third aspect of the present application provides a self-repairing aluminosilicate inorganic glue deep ultraviolet LED packaging method, comprising the following steps:

[0018] Step 1: Printing a self-repairing aluminosilicate inorganic glue as described in any one of the above items on the dam of the ceramic substrate containing the deep ultraviolet LED chip;

[0019] Step 2: placing the quartz glass on the uncured self-repairing aluminosilicate inorganic glue;

[0020] Step 3: Curing the packaged deep ultraviolet LED according to the curing process.

[0021] Furthermore, in the step 1, printing is performed using a screen printer, and the mesh size of the screen printer is 40 to 200. The mesh size of the screen printer should be compatible with the viscosity of the self-repairing aluminosilicate inorganic glue.

[0022] Furthermore, the ceramic substrate is any one of a thin film ceramic substrate, a thick film printed ceramic substrate, a direct bonding ceramic substrate, a direct electroplating ceramic substrate, an active metal welding ceramic substrate, and a laser activated metal ceramic substrate.

[0023] Furthermore, the material of the dam is any one of alumina, aluminum nitride, copper, aluminum, silicate unfired ceramics, phosphate unfired ceramics, and aluminosilicate unfired ceramics.

[0024] Furthermore, the size of the ceramic substrate may be any one of 3.50 mm×3.50 mm, 6.50 mm×6.50 mm, and 6.80 mm×6.80 mm.

[0025] Furthermore, in the step three, the curing temperature of the curing process is 25 to 150°C, and the curing time is 30 to 200 hours. For example, the curing process can be: curing at room temperature for 24 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours, then curing at 150°C for 2 hours; or curing at room temperature for 48 hours, then curing at 90°C for 2 hours, then curing at 150°C for 2 hours; or curing at room temperature for 72 hours, then curing at 150°C for 2 hours; or curing at room temperature for 96 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours; or curing at room temperature for 120 hours, then curing at 50°C for 2 hours; or curing at room temperature for 168 hours. Here, room temperature refers to 25 to 35°C.

[0026] Compared with the prior art, this application has the following technical effects:

[0027] The self-repairing aluminosilicate inorganic adhesive of the present application is an adhesive composed of diamond micropowder, sodium silicate solution and fly ash. The addition of diamond micropowder allows the heat released by the aluminosilicate inorganic adhesive composition during the polycondensation reaction to be stored by diamond, which promotes the transformation of the aluminosilicate inorganic adhesive into a solid body or mineral phase in the diamond-rich area, so that mullite is generated inside the inorganic adhesive at room temperature or slightly above room temperature. The mullite phase grows around the diamond and fills the pores, cracks and other micro-defects inside the inorganic adhesive solid body, thereby promoting the flow of the inorganic adhesive liquid phase, significantly reducing the viscosity of the inorganic adhesive, and realizing the self-repair of the aluminosilicate inorganic adhesive solid body. This increases the density of the aluminosilicate inorganic adhesive solid body, reduces the porosity, and has fewer micro-defects, effectively enhancing its own compressive strength and the shear strength with the copper dam, and improving the airtightness of the packaged deep ultraviolet LED.

[0028] A self-healing aluminosilicate inorganic glue in the present application can achieve self-repair of defect problems of inorganic glue solid body, enhance the self-healing performance of inorganic glue solid body at room temperature or slightly above room temperature, have fewer defects at room temperature or slightly above room temperature, effectively improve the shear strength between the aluminosilicate inorganic glue and the matrix material and the packaging airtightness of the deep ultraviolet LED, and the self-healing behavior of the aluminosilicate inorganic glue can significantly improve the service life and reliability of the deep ultraviolet LED.

[0029] A self-healing aluminosilicate inorganic adhesive of the present application can be used at an operating temperature of room temperature to 1300°C, and has high bonding strength with heterogeneous substrate materials, can be cured at room temperature or slightly above room temperature, has the advantages of resistance to ultraviolet radiation, small molding shrinkage, no pollution to the environment, low production cost, simple preparation process, good processing and molding performance, etc., and is an excellent material to replace encapsulation organic adhesive.

[0030] The present application discloses a self-repairing aluminosilicate inorganic glue deep ultraviolet LED packaging method, which uses self-repairing aluminosilicate inorganic glue as an adhesive, effectively improving the shear strength between the aluminosilicate inorganic glue and the matrix material and the packaging airtightness of the deep ultraviolet LED. The self-repairing behavior of the aluminosilicate inorganic glue can significantly improve the service life and reliability of the deep ultraviolet LED. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0032] Figure 1 This is a scanning electron microscope image of the cured aluminosilicate inorganic glue provided in Example 1 of the present application;

[0033] Figure 2 A scanning electron microscope image of a cured aluminosilicate inorganic glue provided in Example 2 of the present application;

[0034] Figure 3 This is a scanning electron microscope image of the cured aluminosilicate inorganic glue provided in Example 3 of the present application;

[0035] Figure 4 This is a scanning electron microscope image of the cured aluminosilicate inorganic glue provided in Comparative Example 1 of the present application;

[0036] Figure 5 A schematic diagram of a self-repairing aluminosilicate inorganic glue deep ultraviolet LED packaging method provided in an embodiment of the present application.

[0037] Among them, the reference numerals in the figure are:

[0038] 1. Screen printing machine, 2. LED chip, 3. Ceramic substrate, 4. Aluminosilicate inorganic glue, 5. Dam. DETAILED DESCRIPTION

[0039] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present application more clearly understood, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0040] In this application, the term "and / or" describes the association relationship of associated objects, indicating that there may be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone. A and B can be singular or plural. The character " / " generally indicates that the associated objects are in an "or" relationship.

[0041] In the present application, "at least one" means one or more, and "plurality" means two or more. "At least one of the following" or similar expressions refers to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b, or c", or "at least one of a, b, and c" can all represent: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple, respectively.

[0042] The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit the present application. The singular forms "a", "said" and "the" used in the embodiments of the present application and the appended claims are also intended to include plural forms, unless the context clearly indicates other meanings.

[0043] The weight of the relevant components mentioned in the specification of the examples of this application can not only refer to the specific content of each component, but also represent the proportional relationship between the weights of the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the specification of the examples of this application, it is within the scope disclosed in the specification of the examples of this application. Specifically, the mass described in the specification of the examples of this application can be a mass unit known in the biochemical field such as μg, mg, g, kg, etc.

[0044] Embodiment 1

[0045] Embodiment 1 of the present application provides a self-repairing aluminosilicate inorganic adhesive and a deep ultraviolet LED all-inorganic packaging method:

[0046] A self-repairing aluminosilicate inorganic adhesive, the raw materials include: diamond powder, sodium silicate solution, fly ash. Among them, the proportion of diamond powder is 2.70wt%, the proportion of sodium silicate solution is 43.24wt%, and the proportion of fly ash is 54.06wt%. The particle size of diamond powder is 3.5μm, and the impurity content is <0.05wt%; the concentration of sodium silicate solution at room temperature is 40°Bé, composed of 23.83wt% SiO2, 10.25wt% Na2O, and the rest is water; in fly ash, SiO2 accounts for 57.20wt%, Al2O3 accounts for 23.40wt%, Fe2O3 accounts for 6.20wt%, CaO accounts for 5.70wt%, MgO accounts for 2.10wt%, K2O accounts for 2.50wt%, SO3 accounts for 2.1wt%, and the loss on ignition accounts for 0.5wt%. The fly ash includes fly ash with particle sizes of 1.62 μm and 57.65 μm, and the weight ratio of 1.62 μm fly ash to 57.65 μm fly ash is 1:4.

[0047] The self-healing aluminosilicate inorganic glue is prepared by mixing the diamond powder in the raw materials with fly ash through a planetary mixer, and then adding the sodium silicate solution to the powder mixture, which is stirred by a magnetic stirrer until a uniform mixture is obtained at room temperature.

[0048] A self-repairing aluminosilicate inorganic adhesive deep ultraviolet LED packaging method, as shown in the schematic diagram Figure 5 As shown, the following steps are included:

[0049] Step 1: Use a screen printer 1 to print the prepared self-repairing aluminosilicate inorganic glue 4 on the dam 5 of the ceramic substrate 3 containing the deep ultraviolet LED chip 2; the mesh of the screen printer is 80 mesh, the ceramic substrate 3 is a direct electroplating ceramic substrate, the material of the dam 5 is copper, and the size of the ceramic substrate 3 is 3.50 mm×3.50 mm;

[0050] Step 2: Use a vacuum electric suction pen to place the quartz glass on the uncured aluminosilicate inorganic glue 4;

[0051] Step 3: Curing the packaged deep ultraviolet LED chip 2 in a glue baking machine according to the curing process. The curing process is: curing at room temperature for 24 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours, and finally curing at 150°C for 2 hours.

[0052] The viscosity of the aluminosilicate inorganic adhesive prepared in this embodiment, the compressive strength and porosity after curing at room temperature for 7 days in a drying oven, the shear strength with the copper dam, and the airtightness test results of the packaged deep ultraviolet LED are shown in Table 1.

[0053] Embodiment 2

[0054] Embodiment 2 of the present application provides a self-repairing aluminosilicate inorganic adhesive and a deep ultraviolet LED all-inorganic packaging method:

[0055] A self-repairing aluminosilicate inorganic adhesive, the raw materials include: diamond powder, sodium silicate solution, fly ash. Among them, the proportion of diamond powder is 5.26wt%, the proportion of sodium silicate solution is 42.11wt%, and the proportion of fly ash is 52.63wt%. The particle size of diamond powder is 3.5μm, and the impurity content is <0.05wt%; the concentration of sodium silicate solution at room temperature is 40°Bé, composed of 23.83wt% SiO2, 10.25wt% Na2O, and the rest is water; in fly ash, SiO2 accounts for 57.20wt%, Al2O3 accounts for 23.40wt%, Fe2O3 accounts for 6.20wt%, CaO accounts for 5.70wt%, MgO accounts for 2.10wt%, K2O accounts for 2.50wt%, SO3 accounts for 2.1wt%, and the loss on ignition accounts for 0.5wt%. The fly ash includes fly ash with particle sizes of 1.62 μm and 57.65 μm, and the weight ratio of 1.62 μm fly ash to 57.65 μm fly ash is 1:4.

[0056] The self-healing aluminosilicate inorganic glue is prepared by mixing the diamond powder in the raw materials with fly ash through a planetary mixer, and then adding the sodium silicate solution to the powder mixture, which is stirred by a magnetic stirrer until a uniform mixture is obtained at room temperature.

[0057] A self-repairing aluminosilicate inorganic adhesive deep ultraviolet LED packaging method, as shown in the schematic diagram Figure 5 As shown, the following steps are included:

[0058] Step 1: Use a screen printer 1 to print the prepared self-repairing aluminosilicate inorganic glue 4 on the dam 5 of the ceramic substrate 3 containing the deep ultraviolet LED chip 2; the mesh of the screen printer is 100 mesh, the ceramic substrate 3 is a directly electroplated ceramic substrate, the material of the dam 5 is copper, and the size of the ceramic substrate 3 is 3.50 mm×3.50 mm;

[0059] Step 2: Use a vacuum electric suction pen to place the quartz glass on the uncured aluminosilicate inorganic glue 4;

[0060] Step 3: Curing the packaged deep ultraviolet LED chip 2 in a glue baking machine according to the curing process. The curing process is: curing at room temperature for 24 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours, and finally curing at 150°C for 2 hours.

[0061] The viscosity of the aluminosilicate inorganic adhesive prepared in this embodiment, the compressive strength and porosity after curing at room temperature for 7 days in a drying oven, the shear strength with the copper dam, and the airtightness test results of the packaged deep ultraviolet LED are shown in Table 1.

[0062] Embodiment 3

[0063] Embodiment 3 of the present application provides a self-repairing aluminosilicate inorganic adhesive and a deep ultraviolet LED all-inorganic packaging method:

[0064] A self-repairing aluminosilicate inorganic adhesive, the raw materials include: diamond powder, sodium silicate solution, fly ash. Among them, the proportion of diamond powder is 7.69wt%, the proportion of sodium silicate solution is 41.03wt%, and the proportion of fly ash is 51.28wt%. The particle size of diamond powder is 3.5μm, and the impurity content is <0.05wt%; the concentration of sodium silicate solution at room temperature is 40°Bé, composed of 23.83wt% SiO2, 10.25wt% Na2O, and the rest is water; in fly ash, SiO2 accounts for 57.20wt%, Al2O3 accounts for 23.40wt%, Fe2O3 accounts for 6.20wt%, CaO accounts for 5.70wt%, MgO accounts for 2.10wt%, K2O accounts for 2.50wt%, SO3 accounts for 2.1wt%, and the loss on ignition accounts for 0.5wt%. The fly ash includes fly ash with particle sizes of 1.62 μm and 57.65 μm, and the weight ratio of 1.62 μm fly ash to 57.65 μm fly ash is 1:4.

[0065] The self-healing aluminosilicate inorganic glue is prepared by mixing the diamond powder in the raw materials with fly ash through a planetary mixer, and then adding the sodium silicate solution to the powder mixture, which is stirred by a magnetic stirrer until a uniform mixture is obtained at room temperature.

[0066] A self-repairing aluminosilicate inorganic adhesive deep ultraviolet LED packaging method, as shown in the schematic diagram Figure 5 As shown, the following steps are included:

[0067] Step 1: Use a screen printer 1 to print the prepared self-repairing aluminosilicate inorganic glue 4 on the dam 5 of the ceramic substrate 3 containing the deep ultraviolet LED chip 2; the mesh of the screen printer is 150 mesh, the ceramic substrate 3 is a direct electroplating ceramic substrate, the material of the dam 5 is copper, and the size of the ceramic substrate 3 is 3.50 mm×3.50 mm;

[0068] Step 2: Use a vacuum electric suction pen to place the quartz glass on the uncured aluminosilicate inorganic glue 4;

[0069] Step 3: Curing the packaged deep ultraviolet LED chip 2 in a glue baking machine according to the curing process. The curing process is: curing at room temperature for 24 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours, and finally curing at 150°C for 2 hours.

[0070] The viscosity of the aluminosilicate inorganic adhesive prepared in this embodiment, the compressive strength and porosity after curing at room temperature for 7 days in a drying oven, the shear strength with the copper dam, and the airtightness test results of the packaged deep ultraviolet LED are shown in Table 1.

[0071] Comparative Example 1

[0072] Comparative Example 1 of the present application provides a self-repairing aluminosilicate inorganic adhesive and a deep ultraviolet LED all-inorganic packaging method:

[0073] A self-repairing aluminosilicate inorganic adhesive, the raw materials include: sodium silicate solution, fly ash. Among them, the proportion of diamond powder is 0wt%, the proportion of sodium silicate solution is 44.44wt%, and the proportion of fly ash is 55.56wt%. The concentration of sodium silicate solution at room temperature is 40°Bé, and it is composed of 23.83wt% SiO2, 10.25wt% Na2O, and the rest is water; in fly ash, SiO2 accounts for 57.20wt%, Al2O3 accounts for 23.40wt%, Fe2O3 accounts for 6.20wt%, CaO accounts for 5.70wt%, MgO accounts for 2.10wt%, K2O accounts for 2.50wt%, SO3 accounts for 2.1wt%, and the loss on ignition accounts for 0.5wt%. The fly ash includes fly ash with a particle size of 1.62μm and 57.65μm, and the weight ratio of 1.62μm fly ash to 57.65μm fly ash is 1:4.

[0074] The self-healing aluminosilicate inorganic adhesive is prepared by stirring the fly ash and sodium silicate solution in the raw materials by a magnetic stirrer until a uniform mixture is obtained at room temperature.

[0075] A self-repairing aluminosilicate inorganic adhesive deep ultraviolet LED packaging method, as shown in the schematic diagram Figure 5 As shown, the following steps are included:

[0076] Step 1: Use a screen printer 1 to print the prepared self-repairing aluminosilicate inorganic glue 4 on the dam 5 of the ceramic substrate 3 containing the deep ultraviolet LED chip 2; the mesh of the screen printer is 40 mesh, the ceramic substrate 3 is a direct electroplating ceramic substrate, the material of the dam 5 is copper, and the size of the ceramic substrate 3 is 3.50 mm×3.50 mm;

[0077] Step 2: Use a vacuum electric suction pen to place the quartz glass on the uncured aluminosilicate inorganic glue 4;

[0078] Step 3: Curing the packaged deep ultraviolet LED chip 2 in a glue baking machine according to the curing process. The curing process is: curing at room temperature for 24 hours, then curing at 50°C for 2 hours, then curing at 90°C for 2 hours, and finally curing at 150°C for 2 hours.

[0079] The viscosity of the aluminosilicate inorganic adhesive prepared in this comparative example, the compressive strength and porosity after curing at room temperature for 7 days in a drying oven, the shear strength with the copper dam, and the airtightness test results of the packaged deep ultraviolet LED are shown in Table 1.

[0080] Table 1

[0081] Viscosity Compressive strength Porosity Shear Strength Airtightness Embodiment 1 1.40Pa·s 30.14MPa 18.36% 6.74MPa <![CDATA[8.7×10 -7 Pa·m 3 / s]]> Embodiment 2 1.32Pa·s 35.26MPa 11.62% 8.97MPa <![CDATA[4.6×10 -8 Pa·m 3 / s]]> Embodiment 3 1.27Pa·s 27.63MPa 21.51% 6.33MPa <![CDATA[3.5×10 -7 Pa·m 3 / s]]> Comparative Example 1 1.45Pa·s 24.08MPa 28.54% 5.68MPa <![CDATA[6.3×10 -5 Pa·m 3 / s]]>

[0082] The test data of the aluminosilicate inorganic adhesive viscosity provided by Example 1, Example 2, Example 3 and Comparative Example 1, the compressive strength and porosity after curing at room temperature for 7 days in a drying oven, the shear strength with the copper dam, and the airtightness of the packaged deep ultraviolet LED are provided, and Figure 1 , Figure 2 , Figure 3 , Figure 4 By comparing the degree of densification of the microscopic morphology of the aluminosilicate inorganic glue solidified body, it can be found that: in the self-repairing aluminosilicate inorganic glue provided in the embodiment of the present application, the addition of diamond powder allows the heat released by the aluminosilicate inorganic glue composition during the polycondensation reaction to be stored by diamonds, which promotes the transformation of the aluminosilicate inorganic glue in the diamond-rich area to a solidified body or a mineral phase, so that mullite is generated inside the inorganic glue at room temperature or slightly above room temperature. The mullite phase grows around the diamond and fills the pores, cracks and other micro-defects inside the inorganic glue solidified body, thereby promoting the flow of the inorganic glue liquid phase, significantly reducing the viscosity of the inorganic glue, and realizing the self-repair of the aluminosilicate inorganic glue solidified body. This increases the density of the aluminosilicate inorganic glue solidified body, reduces the porosity, and has fewer micro-defects, effectively enhancing its own compressive strength and the shear strength with the copper dam, and improving the airtightness of the packaged deep ultraviolet LED.

[0083] The test results of Example 3 show that when the proportion of diamond micropowder in the aluminosilicate inorganic glue is 7.69wt%, the excessive diamond micropowder hinders the alkali excitation reaction, resulting in incomplete dissolution-depolymerization-condensation reaction of some inorganic glue components, thereby causing a significant increase in the fluidity of the inorganic glue, while its own compressive strength and the shear strength between it and the copper dam of the matrix material will decrease; the porosity increases, causing the airtightness effect of encapsulating deep ultraviolet LEDs to deteriorate.

[0084] Due to the defects such as pores and cracks generated by the aluminosilicate inorganic glue during the alkali excitation reaction, the bonding strength and durability of the aluminosilicate inorganic glue and the matrix material are reduced, and the air tightness, service life and reliability of the deep ultraviolet LED package are seriously affected. The aluminosilicate inorganic glue in the embodiment of the present application can achieve self-repair of the defect problems of the inorganic glue solid body, enhance the self-healing performance of the inorganic glue solid body at room temperature or slightly above room temperature, have fewer defects at room temperature or slightly above room temperature, effectively improve the shear strength between the aluminosilicate inorganic glue and the matrix material and the packaging air tightness of the deep ultraviolet LED, and the self-repairing behavior of the aluminosilicate inorganic glue can significantly improve the service life and reliability of the deep ultraviolet LED.

[0085] The above embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the present application. It should be pointed out that, for a person of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the attached claims.

Claims

1. A self-repairing aluminosilicate inorganic adhesive, characterized in that: Includes the following ingredients: Diamond micro powder 2.7~7.69wt%; the particle size of the diamond micro powder is 3.5 μm, and the impurity content is <0.05wt%; Sodium silicate solution 41~45wt%; the concentration of sodium silicate solution is 40°Bé; Fly ash 51-56wt%; the fly ash is composed of large-size particles and small-size particles, the particle size of the large-size particles is 57.65 μm, the particle size of the small-size particles is 1.62 μm, and the weight ratio of the small-size particles to the large-size particles is 1:

4.

2. A self-repairing aluminosilicate inorganic adhesive as claimed in claim 1, characterized in that: The content of the diamond powder is 5.26wt%~7.69wt%.

3. A self-repairing aluminosilicate inorganic adhesive as claimed in claim 2, characterized in that: The content of the diamond powder is 5.26wt%.

4. A self-repairing aluminosilicate inorganic adhesive as claimed in claim 1, characterized in that: The content of the fly ash is 51.28wt%~52.63wt%.

5. A self-repairing aluminosilicate inorganic adhesive as claimed in claim 4, characterized in that: The content of the fly ash is 52.63wt%.

6. Application of a self-repairing aluminosilicate inorganic adhesive as described in any one of claims 1 to 5 in LED packaging.

7. A method for deep ultraviolet LED packaging using a self-repairing aluminosilicate inorganic adhesive, characterized in that: The following steps are involved: Step 1: Printing the self-repairing aluminosilicate inorganic glue described in any one of claims 1 to 5 above the dam containing the ceramic substrate of the deep ultraviolet LED chip; Step 2: placing the quartz glass on the uncured self-repairing aluminosilicate inorganic glue; Step 3: Curing the packaged deep ultraviolet LED according to the curing process.

8. The method according to claim 7, characterized in that In the step 1, printing is performed using a screen printer, and the screen printing machine has a mesh size of 80 to 150 meshes.

9. The method according to claim 8, characterized in that The ceramic substrate is a direct-bonded ceramic substrate, and the material of the dam is copper.

10. The method according to claim 8, wherein In the step three, the curing temperature of the curing process is 25-150°C, and the curing time is 30-200 h.

Citation Information

Patent Citations

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