CN112625647A - High-heat-resistance LED packaging adhesive and preparation method thereof - Google Patents
High-heat-resistance LED packaging adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The application relates to the technical field of packaging adhesives, and particularly discloses a high-heat-resistance LED packaging adhesive and a preparation method thereof, which solve the problem that the heat resistance of the packaging adhesive is not good in the prior art. The packaging adhesive comprises a component A and a component B in a mass ratio of (0.5-1) to 1; the component A comprises: vinyl silicone oil, phenyl silicone oil, vinyl silicone resin and platinum catalyst; the component B comprises: 0.1-5 parts of dendrimer graphene composite material, 0.5-5 parts of dendrimer gold/silver nanocrystal composite material, vinyl silicone oil, vinyl silicone resin, phenyl silicone oil and hydrogen-containing silicone oil; the dendrimer graphene composite material is obtained by coating graphene in dendrimers, and the dendrimer gold/silver nanocrystal composite material is obtained by loading gold/silver nanocrystals on the dendrimers. The packaging adhesive can be used for packaging LEDs and has the advantage of good thermal stability.
Description
Technical Field
The application relates to the technical field of packaging adhesives, in particular to a high-heat-resistance LED packaging adhesive and a preparation method thereof.
Background
In recent years, with the rapid development of electronic technology, the research on Light Emitting Diode (LED) products has been developed in a breakthrough manner, and the semiconductor device that converts electric energy into light energy has the advantages of rich light emitting color, energy saving, long service life, fast response speed and the like, and is widely applied to the fields of common lighting, traffic signals, landscape lighting, display screens and the like. With the development of LED packaging devices and lighting products towards higher power and higher brightness, higher requirements are also put forward on LED devices and packaging processes thereof, and meanwhile, LED devices and packaging processes thereof are also under continuous innovation and development. Since the LED light emitting chip is disposed in a limited space, increasing the driving current to increase the power of the light source will result in an increase in the amount of heat generated by the LED chip, and thus the requirement for heat resistance of the LED package encapsulant material as an optically transparent window is also increasing.
The LED packaging adhesive is generally made of polymer resin such as silica gel and epoxy, and the polymer resin such as silica gel and epoxy has a defect of poor heat resistance, so that the use of LED packaging devices and lighting products is limited.
Disclosure of Invention
In order to further optimize the problem that the thermal stability of the related LED packaging adhesive is poor, the application provides the high-heat-resistance LED packaging adhesive and the preparation method thereof, and the prepared LED packaging adhesive has the advantage of good heat resistance.
In a first aspect, the application provides a high heat-resistant LED packaging adhesive, which comprises an A component and a B component, wherein the mass ratio of the A component to the B component is (0.5-1): 1;
the component A comprises the following raw materials in parts by weight: 16-28 parts of vinyl silicone oil, 4-17 parts of phenyl silicone oil, 55-80 parts of vinyl silicone resin and 0.1-2 parts of platinum catalyst;
the component B comprises the following raw materials in parts by weight: 0.1-5 parts of dendrimer graphene composite material, 0.5-5 parts of dendrimer gold/silver nanocrystalline composite material, 10-25 parts of vinyl silicone oil, 45-70 parts of vinyl silicone resin, 8-18 parts of phenyl silicone oil and 12-21 parts of hydrogen-containing silicone oil;
the dendrimer graphene composite material is prepared by dispersing graphene and dendrimers in a solvent, dispersing at 0-10 ℃, and removing the solvent;
the dendrimer gold/silver nanocrystal composite material is obtained by loading gold/silver nanocrystals on a dendrimer.
The graphene is loaded on the dendrimer, so that a three-dimensional network structure is formed between the graphene and the dendrimer, and the dendrimer can effectively reduce the agglomeration of the graphene, so that the graphene has better dispersibility in a silica gel system of the component B; in addition, a three-dimensional network structure formed between the graphene and the dendrimer is beneficial to heat dissipation, and when the three-dimensional network structure is used for preparing the packaging adhesive, the heat resistance of the packaging adhesive can be effectively improved.
In the dendrimer gold/silver nanocrystal composite material, gold/silver nanocrystals are attached to dendrimer like leaves to form a three-dimensional heat dissipation network structure; in addition, the dendrimer can also reduce the agglomeration of the gold/silver nanocrystals, enhance the dispersion of the gold/silver nanocrystals in the silica gel system of the component B, and facilitate the heat dissipation of the dendrimer gold/silver nanocrystal composite material.
By adopting the technical scheme, the dendrimer gold/silver nanocrystal composite material and the dendrimer graphene composite material are mixed, the three-dimensional network structures formed by the dendrimer gold/silver nanocrystal composite material and the dendrimer graphene composite material can be mutually crosslinked on the molecular structures, and the formed new three-dimensional network structure can show excellent heat resistance under the synergistic effect of the dendrimer gold/silver nanocrystal composite material and the dendrimer graphene composite material.
Preferably, when the dendrimer-graphene composite material is prepared, the molar ratio of the dendrimer to the graphene is 1 (0.9-5).
By adopting the technical scheme, under the precondition of the raw material dosage ratio, the prepared dendrimer graphene composite material has better dispersibility in a silica gel system of the component B, and is favorable for the heat resistance of the prepared packaging adhesive.
Preferably, the dendrimer gold/silver nanocrystal composite material comprises a dendrimer gold nanocrystal composite material and a dendrimer silver nanocrystal composite material. Further preferably, the dendrimer gold/silver nanocrystal composite material is selected as a dendrimer gold nanocrystal composite material.
Preferably, the preparation of the dendrimer gold nanocrystal composite material comprises the following steps:
dissolving dendrimer in a solvent, dropwise adding a chloroauric acid solution under the stirring condition, and continuously stirring for 0.3-0.8h after mixing is finished to obtain a first mixed solution;
then slowly adding an excessive potassium borohydride solution into the first mixed solution, reacting for 1.5-2.5h, and centrifugally cleaning to obtain the dendrimer gold nanocrystal composite material;
wherein the mass ratio of the chloroauric acid to the dendrimer is 1 (0.1-0.3).
Preferably, the preparation of the dendrimer silver nanocrystal composite material comprises the following steps:
dissolving dendrimer in a solvent, dropwise adding a silver nitrate solution under the stirring condition, and continuously stirring for 0.2-0.8h after the mixing is finished to obtain a second mixed solution;
slowly adding excessive ammonia water into the second mixed solution, reacting for 1.5-2.5h, and centrifugally cleaning to obtain the dendrimer silver nanocrystal composite material;
wherein the molar ratio of silver nitrate to the dendrimer is 1 (0.9-5).
Preferably, the dendrimer is selected from one of PAMAM dendrimer, aryl ether dendrimer and ferrocenyl dendrimer.
Further preferably, the dendrimer is a PAMAM dendrimer.
Compared with aryl ether dendritic molecules and ferrocenyl dendritic molecules, the PAMAM dendrimer has already realized industrial production at present, and the PAMAM dendrimer is selected as one of the raw materials, so that the prepared packaging adhesive has better heat resistance.
In a second aspect, the application provides a preparation method of a high heat resistance LED packaging adhesive, which adopts the following technical scheme:
a preparation method of high heat resistance LED packaging adhesive comprises the following steps:
s1, mixing vinyl silicone oil, phenyl silicone oil, vinyl silicone resin and a platinum catalyst according to the formula of the component A, then adding the dendrimer composite quantum dot composite material, and stirring and mixing uniformly in vacuum under the normal temperature condition to obtain the component A;
s2, according to the formula of the component B, the dendrimer graphene composite material, the dendrimer gold/silver nanocrystalline composite material, the vinyl silicone oil, the vinyl silicone resin, the phenyl silicone oil and the hydrogen-containing silicone oil are stirred and mixed evenly in vacuum under the condition of normal temperature to prepare the component B;
and S3, mixing and curing the component A and the component B according to the mass ratio of (0.5-1) to 1 to prepare the high-heat-resistance LED packaging adhesive.
By adopting the technical scheme.
In summary, the present application has the following beneficial effects:
1. according to the application, the graphene is loaded on the tree-shaped molecules, and the gold/silver nanocrystals are coated on the tree-shaped molecules, so that the dispersion uniformity of the graphene (or the gold/silver nanocrystals) in a packaging adhesive system is enhanced, and the problem of graphene agglomeration is optimized, so that when the graphene is loaded on the tree-shaped molecules and the gold/silver nanocrystals are coated on the tree-shaped molecules for preparing the packaging adhesive, the packaging adhesive obtains better heat resistance.
2. The dendrimer preferably adopted in the application is PAMAM dendrimer, raw materials of which can be obtained commercially, and the industrial production of the packaging adhesive is facilitated.
Detailed Description
The present application will be described in further detail with reference to examples.
Graphene has good optical characteristics and thermal conductivity, and pure defect-free single-layer graphene has a thermal conductivity as high as 5300W/mK, and is the carbon material with the highest thermal conductivity so far.
Metals such as gold and silver also have excellent thermal conductivity, and the quantum effect of metal nanomaterials such as silver nanocrystals and gold nanocrystals can greatly improve the luminous intensity of the fluorescent material.
Therefore, the dendrimer graphene composite material is prepared by loading graphene on the dendrimer, wherein the dendrimer is attached to the graphene, and the dendrimer and the resin system where the dendrimer is located have good compatibility, so that when the graphene is attached to the dendrimer, the possibility of graphene agglomeration is reduced, the dispersion effect of the graphene in the resin system is enhanced, and stronger heat conduction and heat stability are exerted. The dendrimer and the resin system in which the dendrimer is located have good compatibility, when the gold/silver nanocrystal and the dendrimer are mixed, the dispersion effect in the gold/silver nanocrystal resin system is reduced, and the dendrimer gold/silver nanocrystal composite material forms a three-dimensional network heat dissipation structure, so that the dendrimer gold/silver nanocrystal composite material has more excellent heat conduction and thermal stability.
When the packaging adhesive is prepared, the dendrimer graphene composite material and the dendrimer gold/silver nanocrystalline composite material are mixed, and the two composite materials are matched with each other structurally and cooperatively promote the heat resistance of the packaging adhesive.
The raw materials referred to in the present application are generally commercially available unless otherwise specified. PAMAM dendrimer is available from Merck, product specification 536717-5G, PAMAM dendrimer, ethylene diamine core, 6.0 generation solution, molecular weight 58046.11.
Preparation of arylene ether dendrimer
The preparation method of the aromatic ether dendrimer refers to the synthesis of a 1-2 generation aromatic ether dendritic zinc phthalocyanine loaded polymer nanoparticle and the in vitro photodynamic activity [ M ] of the polymer nanoparticle, university of Fujian university, 2011 ].
The method specifically comprises the following steps: in a three-necked flask were added 14.1g (72.0mmol) of p-cyanobenzyl bromide, 4.9g (35.0mmol) of 3, 5-dihydroxybenzyl alcohol, 1.85g (7.0mmol) of 18-C-6 crown ether, 12.1g (87.0mmol) of anhydrous potassium carbonate, 180mL of acetone, and the reaction was vigorously stirred under nitrogen and refluxed for 48 hours. Then filtering, evaporating the solvent under reduced pressure, adding trichloromethane and water for extraction and liquid separation, and taking an organic layer (1); extracting the water layer for three times by using trichloromethane to obtain an organic layer (2); the organic layer (1) and the organic layer (2) were then combined, and the combined organic layers were dried over anhydrous magnesium sulfate to obtain a village product. The crude product was subsequently purified by distillation using n-hexane in a volume ratio of 2: 3: recrystallizing the dichloromethane to obtain 3, 5-di- (4-cyanophenylmethoxy) benzyl alcohol, namely the aromatic ether dendrimer.
Preparation of ferrocenyl dendrimer
The preparation method of the ferrocenyl dendrimer refers to' Lu Bi Ye, Shi Ma Yu, etc.. the synthesis and electrochemical behavior [ J ] of the ferrocenyl dendrimer]Proceedings of south china university, 2009, 37 (12): 28-31 "the specific steps are: dissolving 0.133g (0.723mmol) of methyl 3,4, 5-trihydroxybenzoate in 20mL of DMF, adding 1g of anhydrous potassium carbonate, heating the system to 80 ℃ under the protection of argon, slowly dropwise adding a DMF solution containing 1g (2.385mmol, 10% excess) of 11-ferrocenyl bromoundecane, fully reacting for 24h, filtering while hot, collecting and spin-drying filtrate, and adding CH to the product2Cl2Dissolving, filtering again, collecting and spin-drying filtrate, purifying the crude product by a chromatographic column (eluent is petroleum ether/ethyl acetate with the volume ratio of 10: 1), spin-drying, and removing the solvent in vacuum to obtain the methyl 3,4, 5-tri (11-ferrocenyl) undecyloxy benzoate, namely the ferrocenyl dendrimer.
Preparation example of dendrimer graphene composite
Preparation example 1 of dendrimer graphene composite
In this preparation example, the selected dendrimer is a PAMAM dendrimer, and the specific preparation steps are as follows:
respectively ultrasonically dispersing PAMAM dendrimer and graphene materials in an NMP solvent (N-methyl pyrrolidone), wherein the molar ratio of the PAMAM dendrimer to the graphene is 1:1.3, and respectively obtaining a graphene solution and a PAMAM dendrimer solution; and slowly dropwise adding the graphene solution into the PAMAM dendrimer solution, keeping the temperature at 8-9 ℃ in the dropwise adding process, then ultrasonically dispersing for 1h, and then removing the solvent to obtain the required dendrimer graphene composite material.
The specific method for removing the solvent comprises the following steps: the solution after ultrasonic dispersion was heated to 100 ℃ and then dried under a vacuum of 0.1MPa for 60min, and then distilled under reduced pressure of 0.05MPa while being heated to a flocculent state at 120 ℃.
Preparation example 2 of dendrimer graphene composite
The preparation example and the dendrimer graphene composite material preparation example 1 are different in that the selected dendrimer is an aryl ether dendrimer, and the specific preparation steps are as follows:
respectively ultrasonically dispersing an aromatic ether dendrimer and a graphene material in an NMP solvent (N-methyl pyrrolidone), wherein the molar ratio of the aromatic ether dendrimer to the graphene is 1:0.9, and respectively obtaining a graphene solution and an aromatic ether dendrimer solution; and then slowly dropwise adding the graphene solution into the aromatic ether dendrimer solution, keeping the temperature at 8-9 ℃ in the dropwise adding process, then ultrasonically dispersing for 1h, and then removing the solvent to obtain the required dendrimer graphene composite material.
Preparation example 3 of dendrimer graphene composite
The preparation example and the dendrimer graphene composite material preparation example 1 are different in that the selected dendrimer is a ferrocenyl dendrimer, and the specific preparation steps are as follows:
respectively ultrasonically dispersing a ferrocenyl dendrimer and a graphene material in an NMP solvent (N-methyl pyrrolidone), wherein the molar ratio of the ferrocenyl dendrimer to the graphene is 1:4.2, and respectively obtaining a graphene solution and a ferrocenyl dendrimer solution; and then slowly dropwise adding the graphene solution into the ferrocenyl dendrimer solution, keeping the temperature at 8-9 ℃ in the dropwise adding process, then ultrasonically dispersing for 1h, and then removing the solvent to obtain the required dendrimer graphene composite material.
Preparation example of dendrimer gold/silver nanocrystal composite
Preparation example 1 of dendrimer gold nanocrystal composite
In this preparation example, the selected dendrimer is a PAMAM dendrimer, and the specific preparation steps are as follows:
weighing PAMAM dendrimer, dissolving the PAMAM dendrimer in water, dropwise adding a chloroauric acid solution in stirring at 60r/min, wherein the mass ratio of the chloroauric acid to the PAMAM dendrimer is 1:0.25, and continuously stirring at the same rotating speed for 0.5h after dropwise adding is finished to obtain a mixed solution; then slowly adding excessive potassium borohydride solution into the mixed solution, and reacting for 2 hours; and centrifuging to obtain a solid phase, and cleaning with deionized water to obtain the dendrimer gold nanocrystal composite material.
Preparation example 2 of dendrimer gold nanocrystal composite
The difference between the preparation example and the preparation example 1 of the dendrimer gold nanocrystal composite material is as follows: the selected dendrimer is an aromatic ether dendrimer, and the specific preparation steps are as follows:
weighing and dissolving the aromatic ether dendrimer in water, dropwise adding a chloroauric acid solution in stirring at 10r/min, wherein the mass ratio of the chloroauric acid to the aromatic ether dendrimer is 1:0.25, and continuously stirring at the same rotating speed for 0.5h after dropwise adding is finished to obtain a mixed solution; then slowly adding excessive potassium borohydride solution into the mixed solution, and reacting for 2 hours; and centrifuging to obtain a solid phase, and cleaning with deionized water to obtain the dendrimer gold nanocrystal composite material.
Preparation example 3 of dendrimer gold nanocrystal composite
The difference between the preparation example and the preparation example 1 of the dendrimer gold nanocrystal composite material is as follows: the selected dendrimer is a ferrocenyl dendrimer, and the specific preparation steps are as follows:
weighing ferrocenyl dendrimer, dissolving the ferrocenyl dendrimer in water, dropwise adding a chloroauric acid solution in stirring at 100r/min, wherein the mass ratio of the chloroauric acid to the ferrocenyl dendrimer is 1:0.25, and continuously stirring at the same rotating speed for 0.5h after the dropwise adding is finished to obtain a mixed solution; then slowly adding excessive potassium borohydride solution into the mixed solution, and reacting for 2 hours; and centrifuging to obtain a solid phase, and cleaning with deionized water to obtain the dendrimer gold nanocrystal composite material.
Preparation example of dendrimer silver nanocrystal composite
In this preparation example, the selected dendrimer is a PAMAM dendrimer, and the specific preparation steps are as follows:
weighing PAMAM dendrimer, dissolving in water, dropwise adding a silver nitrate solution under the stirring condition of 80r/min, continuously stirring for 0.5h after mixing is finished, then slowly adding excessive ammonia water into the mixed solution, reacting for 2h, centrifuging, and washing with deionized water to obtain the dendrimer silver nanocrystalline composite material, wherein the molar ratio of silver nitrate to dendrimer is 1: 4.3.
Examples
Example 1
A preparation method of high heat resistance LED packaging adhesive comprises the following steps:
s1, mixing 20g of vinyl silicone oil, 11g of phenyl silicone oil, 67g of vinyl silicone resin and 0.9g of platinum catalyst according to the formula of the component A, then adding 3g of dendrimer quantum dot composite material, and stirring and mixing uniformly in vacuum under the normal temperature condition to obtain the component A;
s2, according to the formula of the component B, uniformly stirring and mixing 2.3g of dendrimer graphene composite material, 2.5g of dendrimer gold nanocrystal composite material, 17g of vinyl silicone oil, 58g of vinyl silicone resin, 12g of phenyl silicone oil and 16g of hydrogen-containing silicone oil in vacuum at normal temperature to obtain the component B;
s3, mixing and curing the component A and the component B according to the mass ratio of 0.6:1 to obtain the high-heat-resistance LED packaging adhesive.
The dendrimer graphene composite material is prepared by the dendrimer graphene composite material preparation example 1; the dendrimer gold nanocrystal composite material is prepared by the dendrimer gold nanocrystal composite material preparation example 2.
Example 2
The difference between this example and example 1 is that the dendrimer graphene composite material selected in this example is prepared by dendrimer graphene composite material preparation example 2, the dendrimer gold nanocrystal composite material is prepared by dendrimer gold nanocrystal composite material preparation example 3, and the others are the same as example 1.
Example 3
The difference between this example and example 1 is that the dendrimer graphene composite material selected in this example is prepared by dendrimer graphene composite material preparation example 3, the dendrimer gold nanocrystal composite material is prepared by dendrimer gold nanocrystal composite material preparation example 1, and the others are the same as example 1.
Example 4
The difference between this example and example 1 is that the dendrimer silver nanocrystal composite material prepared in preparation example 1 of the dendrimer silver nanocrystal composite material is used in this example to replace the dendrimer gold nanocrystal composite material in example 1 in terms of quality, and the other steps are the same as those in example 1.
Example 5
The difference between this example and example 1 is that the gold nanocrystal composite material selected in this example is prepared by dendrimer gold nanocrystal composite material preparation example 3, and the others are the same as example 1.
Examples 6 to 9
Examples 6 to 9 differ from example 1 in the amounts of the respective raw materials used for the preparation of the potting adhesive, as shown in table 1, and the others are the same as example 1.
Table 1 amounts of dendrimer graphene composite and dendrimer gold nanocrystal composite for making encapsulant in examples 6-9
| Item | Dendrimer graphene composite/g | Dendrimer gold nanocrystalline composite/g |
| Example 1 | 2.3 | 2.5 |
| Example 6 | 0.1 | 2.5 |
| Example 7 | 5 | 2.5 |
| Example 8 | 2.3 | 0.5 |
| Example 9 | 2.3 | 5 |
Comparative example 1
The difference between the comparative example and the example 1 is that the raw materials for preparing the encapsulation adhesive in the comparative example do not contain the dendrimer graphene composite, and the rest is the same as the example 1.
Comparative example 2
The difference between the comparative example and the example 1 is that the raw material for preparing the packaging adhesive in the comparative example does not contain the dendrimer gold nanocrystal composite, and the rest is the same as the example 1.
Comparative example 3
The difference between the present comparative example and example 1 is that the raw materials for preparing the encapsulation adhesive in the present comparative example do not contain the dendrimer gold nanocrystal composite material and the dendrimer graphene composite material, and the rest is the same as example 1.
Comparative example 4
The difference between the present comparative example and example 1 is that neither the gold nanocrystal composite material nor the graphene in the raw materials for preparing the encapsulation adhesive in the present comparative example is coated with the dendrimer, and the others are the same as in example 1.
Comparative example 5
The difference between this comparative example and example 1 is that the gold nanocrystalline composite material in the raw material for preparing the encapsulating adhesive in this comparative example is not coated with dendrimer, and the other steps are the same as example 1.
Comparative example 6
The difference between the present comparative example and example 1 is that the graphene in the raw material for preparing the encapsulation adhesive in the present comparative example is not coated with dendrimer, and the other steps are the same as example 1.
Comparative examples 7 to 10
Examples 7 to 10 differ from example 1 in the amounts of the respective raw materials used for the preparation of the potting adhesive, as shown in Table 2, and the others are the same as in example 1.
Table 2 amounts of dendrimer graphene composite and dendrimer gold nanocrystal composite for encapsulation adhesive preparation in comparative examples 7-10
| Item | Dendrimer graphene composite/g | Dendrimer gold nanocrystalline composite/g |
| Example 1 | 2.3 | 2.5 |
| Comparative example 7 | 0.05 | 2.5 |
| Comparative example 8 | 5.5 | 2.5 |
| Comparative example 9 | 2.3 | 0.05 |
| Comparative example 10 | 2.3 | 5.5 |
Performance test
The prepared packaging adhesive is subjected to performance detection, and specific results are shown in table 3.
TABLE 3 Properties of potting adhesive prepared in examples 1 to 9 and comparative examples 1 to 10
The data results in table 3 show that the packaging adhesive prepared by the method has no dead lamp phenomenon under the impact conditions that the cold and hot impact temperature is-40-125 ℃ and 200 rounds. And the dead rate of the packaging adhesive prepared by the comparative example reaches 1-3%. When both the graphene and the gold nanocrystals for preparing the packaging adhesive are not coated with the dendrimer, the dead light rate of the packaging adhesive is the highest and is as high as 3% (data result of comparative example 3).
The yellowing index of the prepared packaging adhesive for 1000 hours is in the range of 1.0-1.6, and is far lower than that of the packaging adhesive in the comparative example by 1.8-4.1; the heat-resistant temperature is in the range of 285-296 ℃, and is far higher than 257-284 ℃ of the comparative example. The data of the comparative examples 1-5 show that the influence of the types of the dendrimer on the yellowing index and the heat-resistant temperature of the prepared packaging adhesive is small, so that the yellowing index of the prepared packaging adhesive is maintained between 1.0 and 1.5, and the heat-resistant temperature is in the range of 287 to 296 ℃; in example 5, the silver nanocrystals are loaded on the dendrimer, and the loading effect of the silver nanocrystals on the dendrimer may be poor, so that the yellowing index of the encapsulation adhesive is slightly higher than that of examples 1 to 4.
It is seen from the data results of comparative examples 1, 6 to 9 and 7 to 10 that, when the encapsulant is prepared, the usage amounts of the dendrimer graphene composite material and the dendrimer gold nanocrystal composite material have an influence on the yellowing index and the heat resistance temperature of the prepared encapsulant: when the dosage of the dendrimer graphene composite material is in the dosage range of 0.1-5 g (embodiment 1, embodiment 6-7) and the dosage of the dendrimer gold nanocrystalline composite material is in the dosage range of 0.5-5 g (embodiment 1, embodiment 8-9), the yellowing index of the packaging adhesive is in the range of 1.0-1.6, and the heat-resistant temperature is changed between 285-289 ℃; when the using amount of the dendrimer graphene composite material is less than 0.1g (comparative example 7), the yellowing index of the packaging adhesive is 2.0, the heat-resistant temperature is 269 ℃, and the yellowing index is obviously higher than that of the packaging adhesive in the embodiment; however, the dosage of the dendrimer graphene composite material is not too much, when the dosage is more than 5g (comparative example 8), the yellowing index of the packaging adhesive is high and is 2.1, the heat-resistant temperature is reduced and is 280 ℃, the dendrimer graphene composite material is possibly too much to be mixed with other raw materials for preparing the packaging adhesive, the three-dimensional network structure is remained, and a compound system with proper cross-linking and matching cannot be completely formed with other raw materials (dendrimer gold nanocrystalline composite material and the like), so that the heat-resistant performance of the packaging adhesive is reduced.
Comparing the data results of comparative example 3 and example 1, it can be seen that the addition of the dendrimer graphene composite and the dendrimer gold nanocrystal composite to the raw materials for preparing the encapsulation adhesive can effectively reduce the dead rate of the encapsulation adhesive, and simultaneously, the yellowing index of the encapsulation adhesive is reduced by 75.6% (from 4.1 to 1.0), and the heat-resistant temperature is increased by 12.5% (257 ℃ to 289 ℃). After the graphene and the gold nanocrystals (comparative example 4) are added in the preparation raw materials, the thermal stability of the packaging adhesive is improved. As can be seen by comparing the data results of comparative examples 5-6 and example 1: the packaging adhesive prepared by adding only the graphene dendrimer composite or only the gold nanocrystal dendrimer composite has low heat resistance (data results of comparative examples 5 and 6), so that the packaging adhesive with better heat resistance and thermal stability can be obtained by adding the graphene dendrimer composite and the gold nanocrystal dendrimer composite at the same time.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The high-heat-resistance LED packaging adhesive is characterized by comprising an A component and a B component, wherein the mass ratio of the A component to the B component is (0.5-1) to 1;
the component A comprises the following raw materials in parts by weight: 16-28 parts of vinyl silicone oil, 4-17 parts of phenyl silicone oil, 55-80 parts of vinyl silicone resin and 0.1-2 parts of platinum catalyst;
the component B comprises the following raw materials in parts by weight: 0.1-5 parts of dendrimer graphene composite material, 0.5-5 parts of dendrimer gold/silver nanocrystalline composite material, 10-25 parts of vinyl silicone oil, 45-70 parts of vinyl silicone resin, 8-18 parts of phenyl silicone oil and 12-21 parts of hydrogen-containing silicone oil;
the dendrimer graphene composite material is prepared by dispersing graphene and dendrimers in a solvent, dispersing at 0-10 ℃, and removing the solvent;
the dendrimer gold/silver nanocrystal composite material is obtained by loading gold/silver nanocrystals on a dendrimer.
2. The LED packaging adhesive with high heat resistance as claimed in claim 1, wherein the molar ratio of the dendrimer to the graphene is 1 (0.9-5) when the dendrimer graphene composite material is prepared.
3. The high heat resistance LED packaging adhesive according to claim 1, wherein: the dendrimer gold/silver nanocrystal composite material comprises a dendrimer gold nanocrystal composite material and a dendrimer silver nanocrystal composite material.
4. The high heat resistance LED packaging adhesive according to claim 3, wherein the preparation of the dendrimer gold nanocrystal composite comprises the following steps:
dissolving dendrimer in a solvent, dropwise adding a chloroauric acid solution under the stirring condition, and continuously stirring for 0.3-0.8h after mixing is finished to obtain a first mixed solution;
then slowly adding an excessive potassium borohydride solution into the first mixed solution, reacting for 1.5-2.5h, and centrifugally cleaning to obtain the dendrimer gold nanocrystal composite material;
wherein the mass ratio of the chloroauric acid to the dendrimer is 1 (0.1-0.3).
5. The high heat resistance LED packaging adhesive according to claim 3, wherein the preparation of the dendrimer silver nanocrystal composite material comprises the following steps:
dissolving dendrimer in a solvent, dropwise adding a silver nitrate solution under the stirring condition, and continuously stirring for 0.2-0.8h after the mixing is finished to obtain a second mixed solution;
slowly adding excessive ammonia water into the second mixed solution, reacting for 1.5-2.5h, and centrifugally cleaning to obtain the dendrimer silver nanocrystal composite material;
wherein the molar ratio of silver nitrate to the dendrimer is 1 (0.9-5).
6. The LED packaging adhesive with high heat resistance of any one of claims 1 to 5, wherein the dendrimer is selected from one of PAMAM dendrimer, aryl ether dendrimer and ferrocenyl dendrimer.
7. The high heat resistance LED packaging adhesive according to claim 6, wherein the dendrimer is a PAMAM dendrimer.
8. The preparation method of the high heat-resistant LED packaging adhesive according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, mixing vinyl silicone oil, phenyl silicone oil, vinyl silicone resin and a platinum catalyst according to the formula of the component A, then adding the dendrimer composite quantum dot composite material, and stirring and mixing uniformly in vacuum under the normal temperature condition to obtain the component A;
s2, according to the formula of the component B, the dendrimer graphene composite material, the dendrimer gold/silver nanocrystalline composite material, the vinyl silicone oil, the vinyl silicone resin, the phenyl silicone oil and the hydrogen-containing silicone oil are stirred and mixed evenly in vacuum under the condition of normal temperature to prepare the component B;
and S3, mixing and curing the component A and the component B according to the mass ratio of (0.5-1) to 1 to prepare the high-heat-resistance LED packaging adhesive.
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