WO2020238261A1 - Encapsulating resin composition for led display screen smt discrete device and application thereof - Google Patents

Encapsulating resin composition for led display screen smt discrete device and application thereof Download PDF

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WO2020238261A1
WO2020238261A1 PCT/CN2020/072357 CN2020072357W WO2020238261A1 WO 2020238261 A1 WO2020238261 A1 WO 2020238261A1 CN 2020072357 W CN2020072357 W CN 2020072357W WO 2020238261 A1 WO2020238261 A1 WO 2020238261A1
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epoxy resin
anhydride
inorganic oxide
polymer particles
organic polymer
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PCT/CN2020/072357
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French (fr)
Chinese (zh)
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谭晓华
于会云
单秋菊
孙绪筠
冯亚凯
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天津德高化成新材料股份有限公司
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Priority to JP2020535013A priority Critical patent/JP7017636B2/en
Publication of WO2020238261A1 publication Critical patent/WO2020238261A1/en

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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
    • 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
    • C09J11/08—Macromolecular additives
    • 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
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
    • G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
    • G09F9/33—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements being semiconductor devices, e.g. diodes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

Definitions

  • the invention relates to an encapsulating resin composition for an LED display screen patch type discrete device and its use.
  • LED devices have gradually tended to be miniaturized, and chip size and lamp bead spacing have been simultaneously reduced.
  • Traditional LED packaging materials show many defects in materials and technology, mainly in the following aspects.
  • the EMC lamp beads emitting light from five sides are smaller in size, and the spacing is closer, and the risk of exposed leads or pins after cutting is greater.
  • the packaging layer becomes thinner the protective effect of the chip gradually weakens. Therefore, it is necessary to strengthen the airtight protection of the chip, which requires the packaging material to have high reliability, especially moisture resistance.
  • traditional packaging materials have poor moisture resistance, resulting in reduced chip reliability.
  • the encapsulating resin is required to have better light decay resistance.
  • the light decay resistance of silicone resin is better than that of epoxy resin, but the hardness of silicone resin is lower, the adhesion to the substrate is smaller, and the air tightness is poor. Therefore, it is difficult to meet the high reliability requirements.
  • ordinary epoxy resins have poor resistance to light decay and are difficult to meet optical requirements.
  • the packaging materials currently used cause uneven light output from each angle of the R, G, and B three-color chips, and the large-angle color has a serious deviation with the viewing angle.
  • the ink color of the screen Inconsistent.
  • the encapsulating resin is required to have good light transmittance.
  • traditional encapsulating materials have high transparency materials and serious warpage; while materials with small warpage have the problem of poor transparency. At present, there is no report to resolve the contradiction between light transmittance and warpage.
  • Chinese Patent CN 105229808 A proposes to add inorganic fillers to solve the warpage problem, which is applied to the reflector material formed by surrounding the metal lead frame and the optical semiconductor element on the optical semiconductor device, rather than the packaging material used to package and protect the chip.
  • the problem solved by the patent is the warpage caused by the bracket itself, rather than the warpage caused by the injection molding of the packaging material.
  • the epoxy resin composition disclosed in this patent needs to have a strong reflective effect, and therefore does not have light transmittance.
  • Patent CN 105518882 A uses light-scattering organic fillers to improve light output efficiency.
  • the used organic filler has an average particle size of 5-15 ⁇ m. If the average particle size is too large, it will be very different from the wavelength of the light wave, which will facilitate the passage of light but reduce the scattering effect.
  • Patent CN 109243313 A mixes melanin with a total weight of 1 ⁇ to 6 ⁇ of epoxy resin to improve the contrast of the display screen. Too much melanin will affect the heat dissipation and light transmittance of LED components. When the amount of melanin added exceeds 0.1%, the brightness of the light-emitting chip drops below 1%, which limits its application in the field of display screens.
  • the purpose of the present invention is to overcome the deficiencies of the prior art, and provide a resin composition for LED display patch type discrete devices with low light decay, warpage resistance, moisture resistance, uniform light output from all angles and high contrast.
  • the second object of the present invention is to provide a use of the encapsulating resin composition for the chip discrete device of the LED display screen.
  • An encapsulating resin composition for LED display screen patch type discrete devices which is characterized by comprising a first type epoxy resin, a second type epoxy resin, acid anhydride, inorganic oxide beads, organic polymer particles and melanin.
  • the mass of the first type epoxy resin is 10 to 61 parts
  • the mass of the second type epoxy resin is 0-60 parts
  • the amount of acid anhydride is the same as the epoxy groups of the first type epoxy resin and the second type epoxy resin.
  • the mass is equal molar ratio
  • the mass of inorganic oxide beads is 5-60 parts
  • the mass of organic polymer particles is the total mass of the first type epoxy resin, second type epoxy resin, acid anhydride and inorganic oxide beads 0.1%-1%
  • the mass of melanin is 0.01%-0.1% of the total mass of the first type epoxy resin, the second type epoxy resin, acid anhydride and inorganic oxide microbeads.
  • the first type epoxy resin is at least one of cycloaliphatic epoxy resin and glycidyl isocyanurate;
  • the cycloaliphatic epoxy resin is poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl formate or CELLOXIDE 8000.
  • the glycidyl isocyanurate is triglycidyl isocyanurate, diglycidyl isocyanurate or monoglycidyl isocyanurate.
  • the second type of epoxy resin is bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin or epoxy silica gel composite epoxy resin.
  • the acid anhydride is tetrahydrophthalic anhydride, phthalic anhydride, trimellitic anhydride, pyromellitic dianhydride, hydrogenated pyromellitic dianhydride, maleic anhydride, methyltetrahydrophthalic anhydride , Hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, nadic anhydride, dodecenyl succinic anhydride, methyl nadic anhydride, hydrogenated methyl nadic anhydride, glutaric anhydride, methyl cyclohexane At least one of enetetracarboxylic dianhydrides.
  • M1 B, Al
  • M2 Mg, Ca, Sr , Zn.
  • the central particle size of the inorganic oxide beads is 5-30 ⁇ m.
  • composition according to claim 1 or 2 wherein the organic polymer particles are at least one of silicone polymer particles, phenol resin particles, polystyrene particles, and polymethyl methacrylate particles,
  • the average particle size of the organic polymer particles is less than 5 ⁇ m.
  • the melanin is at least one of nano carbon black, nano copper oxide and nano manganese oxide.
  • the encapsulating resin composition of the present invention can be applied to a patch type discrete RGB device for display screens.
  • the device includes a five-sided independent light source containing a set of R, G, and B chips, and a module containing 4 sets of RGB chips.
  • the packaging composition of the present invention is applied to the above device packaging, which can improve the moisture resistance, light emission uniformity and contrast of the device, while reducing the warpage generated during the packaging process.
  • the encapsulating resin composition also has the characteristics of low light attenuation for the blue light source in the RGB device, and prolongs the service life of the RGB device.
  • FIG. 1 is a schematic diagram of an LED display screen patch type discrete RGB device encapsulated by the encapsulating resin composition of the present invention.
  • Fig. 2 is a schematic diagram of a front view of a discrete device (4in1) of the LED display screen patch type 4 groups of RGB chip modular light sources encapsulated by the encapsulating resin composition.
  • the components used in the present invention are as follows.
  • the first type of epoxy resin is the first type of epoxy resin.
  • CELLOXIDE 2021P epoxy equivalent 125, Daicel Chemical Industry Co., Ltd., referred to as CELLOXIDE 2021P;
  • Daicel CELLOXIDE 8000 epoxy equivalent is 100, Daicel Chemical Industry Co., Ltd., referred to as CELLOXIDE8000.
  • Triglycidyl isocyanurate, TGIC-D epoxy equivalent of 100, Changzhou Niutang Chemical Factory Co., Ltd., TGIC-D for short.
  • DGIC Diglycidyl isocyanurate, epoxy equivalent 120, referred to as DGIC.
  • MGIC Monoglycidyl isocyanurate, epoxy equivalent 185
  • the second type of epoxy resin is the second type of epoxy resin.
  • JER1002 Bisphenol A epoxy resin, JER1002, epoxy equivalent of 600-700, Mitsubishi Chemical Corporation, referred to as JER1002.
  • Bisphenol A epoxy resin, JER1004, epoxy equivalent is 875 ⁇ 975, Mitsubishi Chemical Corporation, referred to as JER1004.
  • Bisphenol A epoxy resin, JER1007, epoxy equivalent is 1750-2200, Mitsubishi Chemical Corporation, referred to as JER1007.
  • JER1009 Bisphenol A epoxy resin, JER1009, epoxy equivalent of 2400-3300, Mitsubishi Chemical Corporation, referred to as JER1009.
  • Bisphenol A epoxy resin, JER1010, epoxy equivalent is 3000 ⁇ 5000, Mitsubishi Chemical Corporation, JER1010 for short.
  • JER1003F Bisphenol A epoxy resin, JER1003F, epoxy equivalent of 700-800, Mitsubishi Chemical Corporation, referred to as JER1003F.
  • NPES-302 Bisphenol A epoxy resin, NPES-302, epoxy equivalent 600 ⁇ 700, Nanya Plastic Industry Co., Ltd., NPES-302 for short.
  • NPES-303 Bisphenol A epoxy resin, NPES-303, epoxy equivalent 800 ⁇ 900, Nan Ya Plastic Industry Co., Ltd., NPES-303 for short.
  • NPES-304 Bisphenol A epoxy resin, NPES-304, epoxy equivalent 900 ⁇ 1000, Nanya Plastic Industry Co., Ltd., NPES-304 for short.
  • NPES-901 Bisphenol A epoxy resin, NPES-901, epoxy equivalent 450 ⁇ 500, Nanya Plastic Industry Co., Ltd., NPES-901 for short.
  • NPES-902 Bisphenol A epoxy resin, NPES-902, epoxy equivalent 600 ⁇ 650, Nan Ya Plastic Industry Co., Ltd., NPES-902 for short.
  • NPES-904 Bisphenol A epoxy resin, NPES-904, epoxy equivalent 780 ⁇ 850, Nan Ya Plastic Industry Co., Ltd., NPES-904 for short.
  • NPES-905 Bisphenol A epoxy resin, NPES-905, epoxy equivalent of 930 ⁇ 960, Nan Ya Plastic Industry Co., Ltd., referred to as NPES-905.
  • Epoxy silica gel composite epoxy resin epoxy resin:
  • Epoxy silica gel composite epoxy resin ERS-Si1700, epoxy equivalent 200, Mitsubishi Chemical Corporation, abbreviated
  • THPA Tetrahydrophthalic anhydride
  • Phthalic anhydride, acid anhydride equivalent is 148, Nan Ya Plastic Industry Co., Ltd.
  • Trimellitic anhydride has an acid anhydride equivalent of 92.
  • Pyromellitic dianhydride, acid anhydride equivalent is 218, Leheng Chemical Co., Ltd.
  • Hexahydrophthalic anhydride the acid anhydride equivalent is 154, Puyang Huicheng Electronic Materials Co., Ltd.
  • Methyl Nadic acid anhydride the acid anhydride equivalent is 178, Puyang Huicheng Electronic Materials Co., Ltd.
  • Glutaric anhydride, acid anhydride equivalent is 114, Liaoyang Hengye Chemical Co., Ltd.
  • Methylcyclohexene tetracarboxylic dianhydride, anhydride equivalent is 132.
  • Inorganic oxide beads :
  • the preparation method of inorganic oxide microbeads Weigh the raw materials of powder precursors (including oxides, carbonates, hydroxides) of each element according to the target ratio, and after ball milling, mixing, pressure filtering, drying, and then High-temperature sintering, coarse crushing, secondary ball milling, and spray drying to obtain fixed-component inorganic oxide microspheres.
  • Inorganic oxide beads, alumina, center particle size D50 5 ⁇ m, Jiangsu Lianrui New Material Co., Ltd., alumina for short.
  • Inorganic oxide beads, magnesium oxide, center particle size D50 15 ⁇ m, referred to as magnesium oxide.
  • Organic polymer particles KMP-597, silicone polymer particles, with an average particle size of 2 ⁇ m, Shin-Etsu Chemical Co., Ltd., KMP-597 for short.
  • Organic polymer particles KMP-600, silicone polymer particles, average particle size 5 ⁇ m, Shin-Etsu Chemical Co., Ltd., KMP-600 for short.
  • Organic polymer particles KMP-605, silicone polymer particles, with an average particle size of 2 ⁇ m, Shin-Etsu Chemical Co., Ltd., KMP-605 for short.
  • Organic polymer particles X-52-7030, silicone polymer particles, average particle size 0.8 ⁇ m, Shin-Etsu Chemical Co., Ltd., X-52-7030 for short.
  • phenolic resin-1 Organic polymer particles, phenolic resin, with a number average molecular weight of 20,000 to 50,000 and an average particle size of 1um, referred to as phenolic resin-1.
  • phenol resin-2 Organic polymer particles, phenol resin, with a number average molecular weight of 30,000 to 80,000 and an average particle size of 3um, referred to as phenol resin-2.
  • phenolic resin-3 Organic polymer particles, phenolic resin, with a number average molecular weight of 50,000 to 100,000 and an average particle size of 5um, referred to as phenolic resin-3.
  • Polystyrene particles-1 Organic polymer particles, polystyrene particles, with an average particle size of 0.5um, referred to as polystyrene particles-1.
  • Polystyrene particles-2 Organic polymer particles, polystyrene particles, average particle size 2um, referred to as polystyrene particles-2.
  • KM-5030 Organic polymer particles, KM-5030, polystyrene particles, with an average particle size of 3 ⁇ m, Dongguan Kemai New Material Co., Ltd., referred to as KM-5030.
  • Organic polymer particles LD-015, polymethyl methacrylate particles, average particle size 1.5 ⁇ m, Dongguan Xuancheng Chemical Technology Co., Ltd.
  • KMR-3EA Organic polymer particles, KMR-3EA, polymethyl methacrylate particles, with an average particle size of 3 ⁇ m, Japan Soken Chemical Co., Ltd., referred to as KER-3EA.
  • Organic polymer particles KMR-3TA, polymethyl methacrylate particles, with an average particle size of 3 ⁇ m, Japan Soken Chemical Co., Ltd., KMR-3TA for short.
  • the encapsulating resin compositions prepared according to the examples and comparative examples of the present invention will be tested for various properties according to the following methods.
  • Blue light decay Place the hexagonal substrate with blue chip and wire soldered on the mold of the molding equipment, and then preheat and extrude the prepared encapsulating resin composition into the mold cavity through the molding equipment to embed the chip, and expose the hexagonal substrate Wire.
  • the sample needs to be cured at 150°C for 4 hours. Then use the integrating sphere to test the initial luminous flux of the embedded chip when it is lit under a specific current.
  • a series of encapsulating resin compositions to be tested are prepared into samples to be tested according to this method, and then connected in series, lighted continuously with 200mA current (accelerated test) at room temperature for 200 hours, and the remaining luminous flux under a specific current is tested again.
  • Initial luminous flux-remaining luminous flux (Initial luminous flux-remaining luminous flux)/Initial luminous flux, that is, the blue light attenuation of the single sample is obtained.
  • the number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
  • the integrating sphere equipment used in this test is the aluminum base metering integrating sphere R98 manufactured by Hangzhou Yuzhou Optoelectronics Information Co., Ltd.
  • Molding shrinkage rate Weigh 20g of the prepared encapsulating resin composition powder or pellets or block, and inject it into a specific mold at 150°C for curing.
  • the mold cavity is a circle with a diameter of 60mm and a thickness of about 3mm.
  • the number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
  • the mold and injection conditions are the same as the mold shrinkage rate, and the sample with a diameter of 60mm and a thickness of about 3mm is obtained.
  • Continue curing for 4 hours at 150°C. Take out the sample, place it at room temperature, and weigh the sample, which is the initial weight. Then put it into boiling water and continue to boil for 1 hour, take out the sample, wipe off the water, and weigh the quality of the sample. The difference between the two masses divided by the initial mass is the water absorption rate of the sample.
  • the number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
  • Light extraction rate extrude the obtained encapsulating resin composition into a mold with a side length of 30mm and a depth of 0.40mm, cure at 150°C for 2 minutes, and then transfer to an oven at 150°C to continue curing for 4 hours to obtain a side
  • a spectrophotometer to test the light transmittance at 450nm, which is the light output rate.
  • the prepared encapsulating resin composition is encapsulated on a red LED chip by injection molding, and then the radiation intensity distribution data of the chip is tested, that is, the radiation intensity at different angles to determine the light effect.
  • Chip surface temperature Place the hexagonal substrate welded with blue light chips and wires on the mold of the molding equipment, and then preheat and extrude the prepared packaging resin composition into the mold cavity through the molding equipment to embed the chip.
  • the embedding thickness is 1mm, and the wires of the hexagonal substrate are exposed.
  • the sample needs to be cured at 150°C for 4 hours.
  • a series of encapsulating resin compositions to be tested were prepared into samples to be tested according to this method, and then connected in series, with 200mA current (accelerated test) at room temperature for continuous lighting for 1 hour, and an infrared thermal imager was used to test the samples under this condition Chip surface temperature.
  • the blue light attenuation of the single sample is obtained. There are no less than 3 samples for each encapsulation resin composition in a single test, and the average value is taken.
  • An encapsulating resin composition for LED display chip-type discrete devices prepared in the embodiment of the present invention (encapsulating resin composition for short): and the method of preparing the encapsulating resin composition in the comparative example is as follows:
  • the materials were mixed according to the ratio shown in Table 3, mixed uniformly at a temperature of 100° C. using a twin-screw extruder, and then cooled and pulverized to obtain a powdered encapsulating resin composition.
  • the obtained encapsulating resin composition has a significant effect of resisting blue light and light decay.
  • Replacing EHPE-3150 in Example 1 with the first type epoxy resin CELLOXIDE 2021P, CELLOXIDE 8000, DGIC or MGIC can obtain similar blue light resistance performance.
  • Comparative Example 1 since all the second type epoxy resin (JER1002) was used as the main agent, the obtained encapsulating resin composition of the Comparative Example had poor performance against blue light attenuation.
  • the second type epoxy resin including bisphenol A epoxy resin NPES-301, NPES-303, NPES-304, NPES-901, NPES-902, NPES-903, NPES-904, NPES-905, JER1004, JER1007, JER1009, JER1010 and JER1003F; hydrogenated bisphenol A epoxy resin YX-8000, YX-8040, YX-8034 and YL-6753; bisphenol F epoxy resin NPEF-170, NPEF-175, NPEF-176 , NPEF-185, NPEF-187 and NPEF-500; epoxy silica gel composite epoxy resin (ERS-Si1200, ERS-Si1700 and XP833) when JER1002 is replaced, similar blue light resistance performance can be obtained.
  • inorganic oxide beads-7, inorganic oxide beads-8, inorganic oxide beads-9, inorganic oxide beads-10, inorganic oxide beads-11 or inorganic oxide beads-12 instead of implementation
  • inorganic oxide beads-1 in Example 1 a similar effect can be obtained.
  • Comparative Example 3 due to the use of ordinary inorganic oxide microbead silica, although the molding shrinkage rate and water absorption rate of the obtained encapsulating resin composition are also significantly reduced, the light extraction rate is very low, which is lost for light-emitting elements. In addition to the added meaning, it is not suitable for RGB display applications.
  • Comparative Example 1 and Comparative Example 7 it can be found that the encapsulating resin composition still has a certain uniform light emitting effect without using organic polymer particles. Therefore, the inorganic oxide microbeads used in the present invention also have a certain balance of light emission from various angles.
  • the light emission curve shape of the encapsulating resin composition is a smooth arc shape, indicating that the light is uniform at all angles, and the organic polymer particles KMP-590 start To balance the role of light from all angles.
  • the encapsulation resin composition obtained by adding organic polymer microparticle phenol resin-1, KM-503 and KMR-3EA has a smooth arc shape. It shows that the organic polymer microparticle phenolic resin-1, KM-503 and KMR-3EA also have the effect of balancing light emission from various angles.
  • Comparative Example 7 It can be seen from Comparative Example 7 that the encapsulating resin composition without adding organic polymer particles has a large difference in light intensity measured at various angles, the curve shape is zigzag, and the light cannot be emitted uniformly at each angle.
  • polystyrene particles-2, KM-5030, LD-015 and KMR-3TA replace the organic polymer particles KMP-590 in Example 1, the light emission curve of the obtained encapsulating resin composition can achieve a similar effect.
  • Example 2 it can be known from Example 2, Example 7 and Example 8 that when there are more organic polymer particles KMP-590, the water absorption rate of the encapsulating resin composition is significantly increased, and the risk of reliability failure is increased. Therefore, organic polymer particles cannot be used alone, and composite inorganic oxide beads are required to eliminate the risk of increased water absorption.
  • melanin nanometer carbon black 2300# average particle size 15nm
  • melanin nanometer copper oxide average particle size 40nm
  • Example 1 melanin nano-carbon black 2300# average particle size 15nm
  • trimellitic anhydride pyromellitic dianhydride, hydrogenated pyromellitic dianhydride, methyltetrahydrophthalic anhydride, nadic anhydride, dodecenyl succinic anhydride, methyl nadic anhydride, hydrogenated methane
  • kinadic anhydride, glutaric anhydride, and methylcyclohexenetetracarboxylic dianhydride are substituted for maleic anhydride in Example 1, similar effects can be obtained.
  • the encapsulating resin composition for LED display chip discrete devices of the present invention has the characteristics of blue light decay resistance, low water absorption, and increases the airtight protection and reliability of miniaturized and thin devices.
  • the molding shrinkage rate of the epoxy resin composition is reduced, and the warpage after the small-pitch high-density chip packaging is effectively suppressed, and the operability problem of the packaging factory is improved.
  • the encapsulating resin composition of the present invention balances the light intensity of the R, G, and B chips at various angles, so that after the packaged chip set screen is white and balanced on the front side, the color deviation caused by the large angle with the viewing angle disappears.
  • the refined addition of appropriate melanin can improve the contrast without causing the chip temperature to rise.
  • Type I Smooth arc, uniform light intensity at all angles.
  • Class II Zigzag, with huge difference in light intensity from various angles.
  • Type III arc shape with a slight depression in the center angle, and the light intensity at the center angle is slightly lower.
  • the present invention screens out the first and second types of epoxy resin systems, adds acid anhydride, and further introduces inorganic oxide microspheres.
  • the present invention uses selected inorganic oxide microbeads, which have a higher transmittance.
  • the content of the inorganic oxide microbeads accounts for 5-60 parts of the first type epoxy resin, the second type epoxy resin and the inorganic oxide microbeads. Since the thermal conductivity of inorganic oxide microbeads is generally greater than that of epoxy resin, the heat dissipation effect of the composition is also improved to a certain extent.
  • the present invention proposes to add organic polymer particles while adding inorganic oxide beads.
  • the organic polymer particles can mix R, G, and B.
  • the light emitted by the chip can balance the light emitted from various angles at a large angle. For the assembled large-size display, there is no red light when viewed from the side at a large angle after the front white balance is adjusted.
  • the present invention proposes to add melanin to achieve the purpose of improving contrast.
  • the amount of melanin is strictly limited to 0.1% by weight or less .
  • an encapsulating resin composition with low light attenuation, warpage resistance, and moisture resistance is obtained, which can also balance light output, improve contrast and heat dissipation, and enhance end user experience.
  • the thickness of the packaging layer of the LED device packaged in the present invention is generally 0.2-0.6 mm.

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Abstract

The present invention discloses an encapsulating resin composition for LED display screen SMT discrete device and an application thereof, the composition comprises a first-type epoxy resin, a second-type epoxy resin, anhydride, inorganic oxide microbeads, organic polymer particles and melanin. The encapsulating resin composition of the present invention can be applied to a SMT discrete RGB device for display screen, the device comprises a five-sided light-emitting independent light source containing a set of R, G and B chips, and also comprises a modular light source (4in1) containing four sets of RGB chips. The encapsulating composition of the present invention is applied to encapsulating of the above device, moisture resistance, uniformity of light emission and contrast of the device can be improved, and warpage generated during the encapsulating process is reduced. The encapsulating resin composition also has a low light attenuation characteristic for the blue light source in the RGB device, thus prolonging service life of the RGB device.

Description

一种LED显示屏贴片式分立器件用封装树脂组合物及其用途Encapsulation resin composition for LED display screen patch type discrete device and use thereof 技术领域Technical field
本发明涉及一种LED显示屏贴片式分立器件用封装树脂组合物及其用途。The invention relates to an encapsulating resin composition for an LED display screen patch type discrete device and its use.
背景技术Background technique
近些年随着大尺寸显示屏向4K、8K高清显示效果发展，LED器件逐渐倾向于小型化，芯片尺寸和灯珠间距同步缩小。传统的LED封装材料表现出材料和技术诸多缺陷，主要有以下几个方面。In recent years, with the development of large-size display screens to 4K and 8K high-definition display effects, LED devices have gradually tended to be miniaturized, and chip size and lamp bead spacing have been simultaneously reduced. Traditional LED packaging materials show many defects in materials and technology, mainly in the following aspects.
(1)与传统反射杯浇注液体环氧器件相比，五面出光的EMC灯珠尺寸更小，间距更密，切割后的引线或管脚外露的风险更大。而且，随着封装层变薄，对芯片的保护作用逐渐减弱。因此，需要加强对芯片的气密保护性，这就要求封装材料具有较高可靠性，特别是耐潮气性。然而，传统封装材料耐潮气性差，导致芯片可靠性下降。(1) Compared with the traditional reflector cup pouring liquid epoxy device, the EMC lamp beads emitting light from five sides are smaller in size, and the spacing is closer, and the risk of exposed leads or pins after cutting is greater. Moreover, as the packaging layer becomes thinner, the protective effect of the chip gradually weakens. Therefore, it is necessary to strengthen the airtight protection of the chip, which requires the packaging material to have high reliability, especially moisture resistance. However, traditional packaging materials have poor moisture resistance, resulting in reduced chip reliability.
(2)为了满足发光器件尺寸缩小的要求，而采用薄型化基板，传统封装材料容易导致基板明显翘曲，这不利于后续的切割工艺。(2) In order to meet the requirements of reducing the size of the light-emitting device, a thinner substrate is used. Traditional packaging materials are likely to cause obvious warpage of the substrate, which is not conducive to the subsequent cutting process.
(3)对于RGB显示元件，要求封装树脂具有较好的耐光衰特性。有机硅树脂的耐光衰特性优于环氧树脂，但有机硅树脂的硬度较低，对基板的粘结力较小，气密性较差，因此，难以达到高可靠性要求。然而，普通环氧树脂的耐光衰特性差，难以满足光学要求。(3) For RGB display elements, the encapsulating resin is required to have better light decay resistance. The light decay resistance of silicone resin is better than that of epoxy resin, but the hardness of silicone resin is lower, the adhesion to the substrate is smaller, and the air tightness is poor. Therefore, it is difficult to meet the high reliability requirements. However, ordinary epoxy resins have poor resistance to light decay and are difficult to meet optical requirements.
(4)对于显示屏元件，目前使用的封装材料导致R、G、B三色芯片各角度出光不均匀，大角度颜色随视角而产生严重的偏差，而且，RGB芯片组屏后，屏幕的墨色不一致。这些光学缺陷十分明显，从而，制约了RGB器件的广泛应用。(4) For display components, the packaging materials currently used cause uneven light output from each angle of the R, G, and B three-color chips, and the large-angle color has a serious deviation with the viewing angle. Moreover, behind the RGB chip set screen, the ink color of the screen Inconsistent. These optical defects are very obvious, thus restricting the wide application of RGB devices.
(5)作为光半导体元件，要求封装树脂具有较好的透光性，然而，传统封装材料存在透明性高材料，翘曲严重；而翘曲小的材料存在透明性差的问题。目前，还未有报道解决透光性和翘曲之间的矛盾。(5) As an optical semiconductor element, the encapsulating resin is required to have good light transmittance. However, traditional encapsulating materials have high transparency materials and serious warpage; while materials with small warpage have the problem of poor transparency. At present, there is no report to resolve the contradiction between light transmittance and warpage.
对于小型化高密度的显示器应用，提高对比度和散热性也是必然要求。For miniaturized and high-density display applications, improving contrast and heat dissipation are also inevitable requirements.
中国专利CN 105229808 A提出加入无机填充剂解决翘曲问题，其应用于光半导体装置上包围金属引线框和光半导体元件所形成的反射器材料，而不是用于封装保护芯片的封装材料。该专利解决的问题是该反射器所在的支架本身产生的翘曲问题，而不是注塑封装材料后产生的翘曲。该专利所公开的环氧树脂组合物需要具有较强的反射作用，因此不具有透光性。Chinese Patent CN 105229808 A proposes to add inorganic fillers to solve the warpage problem, which is applied to the reflector material formed by surrounding the metal lead frame and the optical semiconductor element on the optical semiconductor device, rather than the packaging material used to package and protect the chip. The problem solved by the patent is the warpage caused by the bracket itself, rather than the warpage caused by the injection molding of the packaging material. The epoxy resin composition disclosed in this patent needs to have a strong reflective effect, and therefore does not have light transmittance.
专利CN 105518882 A使用了光散射性有机填料达到提高光输出效率的目的。为达到其发明目的，所使用的有机填料平均粒径5～15μm。如果平均粒径过大，与光波波长相差悬殊，有利于光的通过，却降低了散射效果。Patent CN 105518882 A uses light-scattering organic fillers to improve light output efficiency. In order to achieve the purpose of the invention, the used organic filler has an average particle size of 5-15 μm. If the average particle size is too large, it will be very different from the wavelength of the light wave, which will facilitate the passage of light but reduce the scattering effect.
专利CN 109243313 A配比了环氧树脂总重量1‰～6‰的黑色素，用以提高显示屏的对比度。黑色素添加量过多，会影响LED元件的散热和透光性。当黑色素添加量超过0.1％时，发光芯片的亮度下降到1％以下，这限制了其在显示屏领域的应用。Patent CN 109243313 A mixes melanin with a total weight of 1‰ to 6‰ of epoxy resin to improve the contrast of the display screen. Too much melanin will affect the heat dissipation and light transmittance of LED components. When the amount of melanin added exceeds 0.1%, the brightness of the light-emitting chip drops below 1%, which limits its application in the field of display screens.
发明内容Summary of the invention
本发明的目的是克服现有技术的不足，提供一种低光衰，抗翘曲，耐潮气，各角度出光均匀和高对比度的LED显示屏贴片式分立器件用封装树脂组合物。The purpose of the present invention is to overcome the deficiencies of the prior art, and provide a resin composition for LED display patch type discrete devices with low light decay, warpage resistance, moisture resistance, uniform light output from all angles and high contrast.
本发明的第二个目的是提供一种LED显示屏贴片式分立器件用封装树脂组合物的用途。The second object of the present invention is to provide a use of the encapsulating resin composition for the chip discrete device of the LED display screen.
本发明的技术方案概述如下：The technical scheme of the present invention is summarized as follows:
一种LED显示屏贴片式分立器件用封装树脂组合物，其特征是包括第一类环氧树脂、第二类环氧树脂、酸酐、无机氧化物微珠、有机聚合物微粒和黑色素。An encapsulating resin composition for LED display screen patch type discrete devices, which is characterized by comprising a first type epoxy resin, a second type epoxy resin, acid anhydride, inorganic oxide beads, organic polymer particles and melanin.
所述第一类环氧树脂的质量为10～61份，第二类环氧树脂的质量为0～60份，酸酐用量与第一类环氧树脂和第二类环氧树脂的环氧基团为等摩尔比，无机氧化物微珠的质量为5～60份，有机聚合物微粒的质量为第一类环氧树脂、第二类环氧树脂、酸酐和无机氧化物微珠总质量的0.1％-1％；黑色素的质量为第一类环氧树脂、第二类环氧树脂、酸酐和无机氧化物微珠总质量的0.01％～0.1％。The mass of the first type epoxy resin is 10 to 61 parts, the mass of the second type epoxy resin is 0-60 parts, and the amount of acid anhydride is the same as the epoxy groups of the first type epoxy resin and the second type epoxy resin. The mass is equal molar ratio, the mass of inorganic oxide beads is 5-60 parts, and the mass of organic polymer particles is the total mass of the first type epoxy resin, second type epoxy resin, acid anhydride and inorganic oxide beads 0.1%-1%; the mass of melanin is 0.01%-0.1% of the total mass of the first type epoxy resin, the second type epoxy resin, acid anhydride and inorganic oxide microbeads.
所述第一类环氧树脂为脂环族环氧树脂、异氰尿酸缩水甘油酯中的至少一种；The first type epoxy resin is at least one of cycloaliphatic epoxy resin and glycidyl isocyanurate;
所述脂环族环氧树脂为聚[(2-环氧乙烷基)-1,2-环己二醇]2-乙基-2-(羟甲基)-1,3-丙二醇醚、3,4-环氧环己基甲基3,4-环氧环己基甲酸酯或大赛璐CELLOXIDE 8000。The cycloaliphatic epoxy resin is poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 3,4-epoxycyclohexyl methyl 3,4-epoxycyclohexyl formate or CELLOXIDE 8000.
所述异氰尿酸缩水甘油酯为异氰尿酸三缩水甘油酯、异氰尿酸二缩水甘油酯或异氰尿酸单缩水甘油酯。The glycidyl isocyanurate is triglycidyl isocyanurate, diglycidyl isocyanurate or monoglycidyl isocyanurate.
所述第二类环氧树脂为双酚A型环氧树脂、氢化双酚A型环氧树脂、双酚F型环氧树脂或环氧硅胶复合环氧树脂。The second type of epoxy resin is bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol F epoxy resin or epoxy silica gel composite epoxy resin.
所述酸酐为四氢苯二甲酸酐、苯二甲酸酐、偏苯三甲酸酐、均苯四甲酸二酐、氢化均苯四甲酸二酐、顺丁烯二酸酐、甲基四氢苯二甲酸酐、六氢苯二甲酸酐、甲基六氢苯二甲酸酐、纳迪克酸酐、十二烯基丁二酸酐、甲基纳迪克酸酐、氢化甲基纳迪克酸酐、戊二酸酐、甲基环己烯四羧酸二酐中至少一种。The acid anhydride is tetrahydrophthalic anhydride, phthalic anhydride, trimellitic anhydride, pyromellitic dianhydride, hydrogenated pyromellitic dianhydride, maleic anhydride, methyltetrahydrophthalic anhydride , Hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, nadic anhydride, dodecenyl succinic anhydride, methyl nadic anhydride, hydrogenated methyl nadic anhydride, glutaric anhydride, methyl cyclohexane At least one of enetetracarboxylic dianhydrides.
所述无机氧化物微珠的通式为Na(1-x-y-z-u)O(1-x-y-z-u)/2·SixO2x·M1yO3y/2·M2zOz·ZruO2u，其中M1＝B、Al；M2＝Mg、Ca、Sr、Zn。 对各元素的含量，0.4≤x≤0.7；0.1≤y≤0.3；z≤0.3；u≤0.3；x+y+z+u≥0.9，其中z、u与1-x-y-z-u不能同时为零，所述无机氧化物微珠的中心粒径为5～30μm。The general formula of the inorganic oxide beads is Na(1-xyzu)O(1-xyzu)/2·SixO2x·M1yO3y/2·M2zOz·ZruO2u, where M1=B, Al; M2=Mg, Ca, Sr , Zn. For the content of each element, 0.4≤x≤0.7; 0.1≤y≤0.3; z≤0.3; u≤0.3; x+y+z+u≥0.9, where z, u and 1-xyzu cannot be zero at the same time, so The central particle size of the inorganic oxide beads is 5-30 μm.
7.根据权利要求1或2所述的组合物，其特征是所述有机聚合物微粒为有机硅聚合物微粒酚醛树脂微粒、聚苯乙烯微粒和聚甲基丙烯酸甲酯微粒中至少一种，所述有机聚合物微粒平均粒径在5μm以下。7. The composition according to claim 1 or 2, wherein the organic polymer particles are at least one of silicone polymer particles, phenol resin particles, polystyrene particles, and polymethyl methacrylate particles, The average particle size of the organic polymer particles is less than 5 μm.
所述黑色素为纳米炭黑、纳米氧化铜和纳米氧化锰中至少一种。The melanin is at least one of nano carbon black, nano copper oxide and nano manganese oxide.
上述组合物在LED显示屏贴片式RGB分立器件封装的应用。Application of the above-mentioned composition in the packaging of LED display screen chip RGB discrete devices.
本发明的优点：Advantages of the invention:
1)降低翘曲；1) Reduce warpage;
2)使耐潮气性有明显提升；2) Obviously improve the moisture resistance;
3)具有一定光散射作用，达到光型配光效果；3) It has a certain light scattering effect to achieve the light-type light distribution effect;
4)具有提升复合物导热率的效果；4) It has the effect of improving the thermal conductivity of the composite;
5)具有提高LED器件对比度的效果；5) It has the effect of improving the contrast of LED devices;
6)提升以上所诉性能的同时，使元件仍然保持良好的透过率。6) While improving the performance described above, the component still maintains a good transmittance.
本发明的封装树脂组合物可以应用在显示屏用的贴片式分立RGB器件中，该器件包括含有一组R、G、B芯片的五面出光独立光源，也包括含有4组RGB芯片的模块化光源(4in1)。本发明的封装组合物应用于以上的器件封装，可以提高器件的耐潮气性、出光均匀性和提高对比度，同时降低封装过程中产生的翘曲。本封装树脂组合物对RGB器件中的蓝光光源，还具有低光衰的特性，延长RGB器件的使用寿命。The encapsulating resin composition of the present invention can be applied to a patch type discrete RGB device for display screens. The device includes a five-sided independent light source containing a set of R, G, and B chips, and a module containing 4 sets of RGB chips. Chemical light source (4in1). The packaging composition of the present invention is applied to the above device packaging, which can improve the moisture resistance, light emission uniformity and contrast of the device, while reducing the warpage generated during the packaging process. The encapsulating resin composition also has the characteristics of low light attenuation for the blue light source in the RGB device, and prolongs the service life of the RGB device.
附图说明Description of the drawings
图1为使用本发明的封装树脂组合物封装的LED显示屏贴片式分立RGB器件示意图。FIG. 1 is a schematic diagram of an LED display screen patch type discrete RGB device encapsulated by the encapsulating resin composition of the present invention.
图2为使用封装树脂组合物封装的LED显示屏贴片式4组RGB芯片模块化光源的分立器件(4in1)主视图的示意图。Fig. 2 is a schematic diagram of a front view of a discrete device (4in1) of the LED display screen patch type 4 groups of RGB chip modular light sources encapsulated by the encapsulating resin composition.
具体实施方式Detailed ways
下面结合具体实施例对本发明作进一步的说明。The present invention will be further described below in conjunction with specific embodiments.
本发明中使用的各成分物质如下。The components used in the present invention are as follows.
第一类环氧树脂：The first type of epoxy resin:
脂环族环氧树脂Alicyclic epoxy resin
聚[(2-环氧乙烷基)-1,2-环己二醇]2-乙基-2-(羟甲基)-1,3-丙二醇醚，商品名EHPE-3150，环氧当量为177，大赛璐化学工业株式会社，简称EHPE-3150；Poly[(2-Ethylene oxide)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, trade name EHPE-3150, epoxy equivalent 177, Daicel Chemical Industry Co., Ltd., referred to as EHPE-3150;
3,4-环氧环己基甲基3,4-环氧环己基甲酸酯，商品名CELLOXIDE 2021P，环氧当量为125，大赛璐化学工业株式会社，简称CELLOXIDE 2021P；3,4-Epoxycyclohexylmethyl 3,4-epoxycyclohexylcarboxylate, trade name CELLOXIDE 2021P, epoxy equivalent 125, Daicel Chemical Industry Co., Ltd., referred to as CELLOXIDE 2021P;
大赛璐CELLOXIDE 8000，环氧当量为100，大赛璐化学工业株式会社，简称CELLOXIDE8000。Daicel CELLOXIDE 8000, epoxy equivalent is 100, Daicel Chemical Industry Co., Ltd., referred to as CELLOXIDE8000.
异氰尿酸缩水甘油酯：Glycidyl isocyanurate:
异氰尿酸三缩水甘油酯，TGIC-D，环氧当量为100，常州市牛塘化工厂有限公司，简称TGIC-D。Triglycidyl isocyanurate, TGIC-D, epoxy equivalent of 100, Changzhou Niutang Chemical Factory Co., Ltd., TGIC-D for short.
异氰尿酸二缩水甘油酯，环氧当量120，简称DGIC。Diglycidyl isocyanurate, epoxy equivalent 120, referred to as DGIC.
异氰尿酸单缩水甘油酯，环氧当量185，简称MGIC。Monoglycidyl isocyanurate, epoxy equivalent 185, referred to as MGIC.
第二类环氧树脂：The second type of epoxy resin:
双酚A型环氧树脂：Bisphenol A type epoxy resin:
双酚A型环氧树脂，JER1002，环氧当量为600～700，三菱化学株式会社，简称JER1002。Bisphenol A epoxy resin, JER1002, epoxy equivalent of 600-700, Mitsubishi Chemical Corporation, referred to as JER1002.
双酚A型环氧树脂，JER1004，环氧当量为875～975，三菱化学株式会社，简称JER1004。Bisphenol A epoxy resin, JER1004, epoxy equivalent is 875～975, Mitsubishi Chemical Corporation, referred to as JER1004.
双酚A型环氧树脂，JER1007，环氧当量为1750～2200，三菱化学株式会社，简称JER1007。Bisphenol A epoxy resin, JER1007, epoxy equivalent is 1750-2200, Mitsubishi Chemical Corporation, referred to as JER1007.
双酚A型环氧树脂，JER1009，环氧当量为2400～3300，三菱化学株式会社，简称JER1009。Bisphenol A epoxy resin, JER1009, epoxy equivalent of 2400-3300, Mitsubishi Chemical Corporation, referred to as JER1009.
双酚A型环氧树脂，JER1010，环氧当量为3000～5000，三菱化学株式会社，简称JER1010。Bisphenol A epoxy resin, JER1010, epoxy equivalent is 3000～5000, Mitsubishi Chemical Corporation, JER1010 for short.
双酚A型环氧树脂，JER1003F，环氧当量为700～800，三菱化学株式会社，简称JER1003F。Bisphenol A epoxy resin, JER1003F, epoxy equivalent of 700-800, Mitsubishi Chemical Corporation, referred to as JER1003F.
双酚A型环氧树脂，NPES-301，环氧当量450～500，南亚塑胶工业股份有限公司，简称NPES-301。Bisphenol A epoxy resin, NPES-301, epoxy equivalent 450～500, Nan Ya Plastic Industry Co., Ltd., NPES-301 for short.
双酚A型环氧树脂，NPES-302，环氧当量600～700，南亚塑胶工业股份有限公司，简称NPES-302。Bisphenol A epoxy resin, NPES-302, epoxy equivalent 600～700, Nanya Plastic Industry Co., Ltd., NPES-302 for short.
双酚A型环氧树脂，NPES-303，环氧当量800～900，南亚塑胶工业股份有限公司，简称NPES-303。Bisphenol A epoxy resin, NPES-303, epoxy equivalent 800~900, Nan Ya Plastic Industry Co., Ltd., NPES-303 for short.
双酚A型环氧树脂，NPES-304，环氧当量900～1000，南亚塑胶工业股份有限公司，简称NPES-304。Bisphenol A epoxy resin, NPES-304, epoxy equivalent 900～1000, Nanya Plastic Industry Co., Ltd., NPES-304 for short.
双酚A型环氧树脂，NPES-901，环氧当量450～500，南亚塑胶工业股份有限公司，简称NPES-901。Bisphenol A epoxy resin, NPES-901, epoxy equivalent 450～500, Nanya Plastic Industry Co., Ltd., NPES-901 for short.
双酚A型环氧树脂，NPES-902，环氧当量600～650，南亚塑胶工业股份有限公司，简称NPES-902。Bisphenol A epoxy resin, NPES-902, epoxy equivalent 600～650, Nan Ya Plastic Industry Co., Ltd., NPES-902 for short.
双酚A型环氧树脂，NPES-903，环氧当量70～750，南亚塑胶工业股份有限公司，简称NPES-903。Bisphenol A epoxy resin, NPES-903, epoxy equivalent 70～750, Nan Ya Plastic Industry Co., Ltd., NPES-903 for short.
双酚A型环氧树脂，NPES-904，环氧当量780～850，南亚塑胶工业股份有限公司，简称NPES-904。Bisphenol A epoxy resin, NPES-904, epoxy equivalent 780～850, Nan Ya Plastic Industry Co., Ltd., NPES-904 for short.
双酚A型环氧树脂，NPES-905，环氧当量930～960，南亚塑胶工业股份有限公司，简称NPES-905。Bisphenol A epoxy resin, NPES-905, epoxy equivalent of 930～960, Nan Ya Plastic Industry Co., Ltd., referred to as NPES-905.
氢化双酚A型环氧树脂：Hydrogenated bisphenol A epoxy resin:
氢化双酚A型环氧树脂，YX-8000，环氧当量205，三菱化学株式会社，简称YX-8000。Hydrogenated bisphenol A epoxy resin, YX-8000, epoxy equivalent 205, Mitsubishi Chemical Corporation, YX-8000 for short.
氢化双酚A型环氧树脂，YX-8040，环氧当量1000，三菱化学株式会社，简称YX-8040。Hydrogenated bisphenol A epoxy resin, YX-8040, epoxy equivalent 1000, Mitsubishi Chemical Corporation, YX-8040 for short.
氢化双酚A型环氧树脂，YX-8034，环氧当量290，三菱化学株式会社，简称YX-8034。Hydrogenated bisphenol A epoxy resin, YX-8034, epoxy equivalent 290, Mitsubishi Chemical Corporation, YX-8034 for short.
氢化双酚A型环氧树脂，YL-6753，环氧当量180，三菱化学株式会社，简称YL-6753。Hydrogenated bisphenol A epoxy resin, YL-6753, epoxy equivalent 180, Mitsubishi Chemical Corporation, YL-6753 for short.
双酚F型环氧树脂：Bisphenol F type epoxy resin:
双酚F型环氧树脂，NPEF-170，环氧当量160～180，南亚塑胶工业股份有限公司，简称NPEF-170。Bisphenol F epoxy resin, NPEF-170, epoxy equivalent 160～180, Nanya Plastic Industry Co., Ltd., NPEF-170 for short.
双酚F型环氧树脂，NPEF-175，环氧当量160～180，南亚塑胶工业股份有限公司，简称NPEF-175。Bisphenol F epoxy resin, NPEF-175, epoxy equivalent 160～180, Nanya Plastic Industry Co., Ltd., NPEF-175 for short.
双酚F型环氧树脂，NPEF-176，环氧当量170～190，南亚塑胶工业股份有限公司，简称NPEF-176。Bisphenol F epoxy resin, NPEF-176, epoxy equivalent 170～190, Nanya Plastic Industry Co., Ltd., NPEF-176 for short.
双酚F型环氧树脂，NPEF-185，环氧当量170～190，南亚塑胶工业股份有限公司，简称NPEF-185。Bisphenol F epoxy resin, NPEF-185, epoxy equivalent 170～190, Nanya Plastic Industry Co., Ltd., NPEF-185 for short.
双酚F型环氧树脂，NPEF-187，环氧当量175～185，南亚塑胶工业股份有限公司，简称NPEF-187。Bisphenol F epoxy resin, NPEF-187, epoxy equivalent 175～185, Nan Ya Plastic Industry Co., Ltd., NPEF-187 for short.
双酚F型环氧树脂，NPEF-500，环氧当量164～170，南亚塑胶工业股份有限公司，简称NPEF-500。Bisphenol F epoxy resin, NPEF-500, epoxy equivalent of 164～170, Nanya Plastic Industry Co., Ltd., NPEF-500 for short.
环氧硅胶复合环氧树脂：Epoxy silica gel composite epoxy resin:
环氧硅胶复合环氧树脂，ERS-Si1200，环氧当量1100～1200，三菱化学株式会社，简称ERS-Si1200。Epoxy silica gel composite epoxy resin, ERS-Si1200, epoxy equivalent 1100~1200, Mitsubishi Chemical Corporation, referred to as ERS-Si1200.
环氧硅胶复合环氧树脂，ERS-Si1700，环氧当量200，三菱化学株式会社，简称Epoxy silica gel composite epoxy resin, ERS-Si1700, epoxy equivalent 200, Mitsubishi Chemical Corporation, abbreviated
ERS-Si1700。ERS-Si1700.
环氧硅胶复合环氧树脂，XP833，环氧当量300，三菱化学株式会社，简称XP833。Epoxy silica gel composite epoxy resin, XP833, epoxy equivalent 300, Mitsubishi Chemical Corporation, referred to as XP833.
酸酐：Anhydride:
四氢苯二甲酸酐(THPA)，酸酐当量为152，南亚塑胶工业股份有限公司，简称THPA。Tetrahydrophthalic anhydride (THPA), with an acid anhydride equivalent of 152, Nan Ya Plastic Industry Co., Ltd., referred to as THPA.
苯二甲酸酐，酸酐当量为148，南亚塑胶工业股份有限公司。Phthalic anhydride, acid anhydride equivalent is 148, Nan Ya Plastic Industry Co., Ltd.
偏苯三甲酸酐，酸酐当量为92。Trimellitic anhydride has an acid anhydride equivalent of 92.
均苯四甲酸二酐，酸酐当量为218，乐恒化工有限公司。Pyromellitic dianhydride, acid anhydride equivalent is 218, Leheng Chemical Co., Ltd.
氢化均苯四甲酸二酐，酸酐当量为224。Hydrogenated pyromellitic dianhydride, anhydride equivalent of 224.
顺丁烯二酸酐，酸酐当量为98。Maleic anhydride with an acid anhydride equivalent of 98.
甲基四氢苯二甲酸酐，酸酐当量为166，濮阳惠成电子材料股份有限公司。Methyltetrahydrophthalic anhydride, anhydride equivalent of 166, Puyang Huicheng Electronic Materials Co., Ltd.
六氢苯二甲酸酐，酸酐当量为154，濮阳惠成电子材料股份有限公司。Hexahydrophthalic anhydride, the acid anhydride equivalent is 154, Puyang Huicheng Electronic Materials Co., Ltd.
甲基六氢苯二甲酸酐，酸酐当量为168，濮阳惠成电子材料股份有限公司。Methyl hexahydrophthalic anhydride, anhydride equivalent of 168, Puyang Huicheng Electronic Materials Co., Ltd.
纳迪克酸酐，酸酐当量为164，濮阳惠成电子材料股份有限公司。Nadic acid anhydride, anhydride equivalent of 164, Puyang Huicheng Electronic Materials Co., Ltd.
十二烯基丁二酸酐，酸酐当量为266，濮阳惠成电子材料股份有限公司。Dodecenyl succinic anhydride, anhydride equivalent of 266, Puyang Huicheng Electronic Materials Co., Ltd.
甲基纳迪克酸酐，酸酐当量为178，濮阳惠成电子材料股份有限公司。Methyl Nadic acid anhydride, the acid anhydride equivalent is 178, Puyang Huicheng Electronic Materials Co., Ltd.
氢化甲基纳迪克酸酐，酸酐当量为180，濮阳惠成电子材料股份有限公司。Hydrogenated methyl Nadic acid anhydride with an acid anhydride equivalent of 180, Puyang Huicheng Electronic Materials Co., Ltd.
戊二酸酐，酸酐当量为114，辽阳恒业化工有限公司。Glutaric anhydride, acid anhydride equivalent is 114, Liaoyang Hengye Chemical Co., Ltd.
甲基环己烯四羧酸二酐，酸酐当量为132。Methylcyclohexene tetracarboxylic dianhydride, anhydride equivalent is 132.
无机氧化物微珠：Inorganic oxide beads:
无机氧化物微珠-1，其化学组成为Si0.55O1.1·B0.2O0.3·Ca0.15O0.15·Zr0.1O0.2，中心粒径D50＝20μm，简称无机氧化物微珠-1。Inorganic oxide microbeads-1, its chemical composition is Si0.55O1.1·B0.2O0.3·Ca0.15O0.15·Zr0.1O0.2, and the central particle size is D50=20μm, referred to as inorganic oxide beads- 1.
无机氧化物微珠-2，其化学组成为Na0.1O0.05·Si0.5O1.0·B0.1O0.15·Zr0.3O0.6，中心粒径D50＝10μm，简称无机氧化物微珠-2。Inorganic oxide microbeads-2, its chemical composition is Na0.1O0.05·Si0.5O1.0·B0.1O0.15·Zr0.3O0.6, and the central particle size is D50=10μm, referred to as inorganic oxide beads- 2.
无机氧化物微珠-3，其化学组成为Na0.04O0.02·Si0.6O1.2·B0.16O0.24·Zr0.2O0.4，中心粒径D50＝5μm，，简称无机氧化物微珠-3。Inorganic oxide beads-3, its chemical composition is Na0.04O0.02·Si0.6O1.2·B0.16O0.24·Zr0.2O0.4, and the central particle size is D50=5μm, referred to as inorganic oxide beads -3.
无机氧化物微珠-4，其化学组成为Si0.4O0.8·Al0.3O0.45·Ca0.1O0.1·Mg0.2O0.2，中心粒径D50＝12μm，简称无机氧化物微珠-4。Inorganic oxide beads-4, its chemical composition is Si0.4O0.8·Al0.3O0.45·Ca0.1O0.1·Mg0.2O0.2, and the central particle size is D50=12μm, referred to as inorganic oxide beads- 4.
无机氧化物微珠-5，其化学组成为Si0.6O1.2·Al0.1O0.15·Ca0.2O0.2·Zn0.1O0.1，中心粒径D50＝15μm，简称无机氧化物微珠-5。Inorganic oxide microbeads-5, its chemical composition is Si0.6O1.2·Al0.1O0.15·Ca0.2O0.2·Zn0.1O0.1, and the central particle size D50=15μm, referred to as inorganic oxide beads- 5.
无机氧化物微珠-6，其化学组成为Na0.06O0.03·Si0.56O1.12·Al0.28O0.42·Ca0.1O0.1，中心粒径D50＝25μm，简称无机氧化物微珠-6。Inorganic oxide microbeads-6, its chemical composition is Na0.06O0.03·Si0.56O1.12·Al0.28O0.42·Ca0.1O0.1, the central particle size is D50=25μm, referred to as inorganic oxide microbeads- 6.
无机氧化物微珠-7，其化学组成为Si0.7O1.4·Al0.05O0.075·B0.15O0.225·Mg0.1O0.1，中心粒径D50＝30μm，简称无机氧化物微珠-7。Inorganic oxide microbeads-7, its chemical composition is Si0.7O1.4·Al0.05O0.075·B0.15O0.225·Mg0.1O0.1, and the central particle size is D50=30μm, referred to as inorganic oxide beads- 7.
无机氧化物微珠-8，其化学组成为Si0.45O0.9·Al0.2O0.3·B0.1O0.15·Ca0.15O0.15·Zn0.1O0.1，中心粒径D50＝8μm，简称无机氧化物微珠-8。Inorganic oxide microbeads-8, its chemical composition is Si0.45O0.9·Al0.2O0.3·B0.1O0.15·Ca0.15O0.15·Zn0.1O0.1, the center particle diameter D50=8μm, abbreviated Inorganic oxide beads-8.
无机氧化物微珠-9，其化学组成为Na0.04O0.02·Si0.6O1.2·Al0.1O0.15·Ca0.26O0.26，中心粒径D50＝25μm，简称无机氧化物微珠-9。Inorganic oxide microbeads-9, its chemical composition is Na0.04O0.02·Si0.6O1.2·Al0.1O0.15·Ca0.26O0.26, and the central particle size is D50=25μm, referred to as inorganic oxide beads- 9.
无机氧化物微珠-10，其化学组成为Si0.5O1.0·B0.3O0.45·Mg0.1O0.1·Sr0.1O0.1，中心粒径D50＝15μm，简称无机氧化物微珠-10。Inorganic oxide microbeads-10, its chemical composition is Si0.5O1.0·B0.3O0.45·Mg0.1O0.1·Sr0.1O0.1, and the central particle size is D50=15μm, referred to as inorganic oxide beads- 10.
无机氧化物微珠-11，其化学组成为Si0.6O1.2·Al0.2O0.3·Mg0.15O0.15·Sr0.05O0.05，中心粒径D50＝24μm，简称无机氧化物微珠-11。Inorganic oxide beads-11, its chemical composition is Si0.6O1.2·Al0.2O0.3·Mg0.15O0.15·Sr0.05O0.05, and the central particle size D50=24μm, referred to as inorganic oxide beads- 11.
无机氧化物微珠-12，其化学组成为Si0.6O1.2·Al0.2O0.3·Zr0.2O0.4，中心粒径D50＝30μm，简称无机氧化物微珠-12。Inorganic oxide microbeads-12, its chemical composition is Si0.6O1.2·Al0.2O0.3·Zr0.2O0.4, and the central particle size is D50=30μm, referred to as inorganic oxide microbeads-12.
无机氧化物微珠的制备方法：按照目标配比称量各元素的粉状前体(包括氧化物、碳酸盐、氢氧化物)原料，经球磨、混合、压滤、干燥后，再经高温烧结、粗粉碎、二次球磨、喷雾干燥，得到固定成分的无机氧化物微珠。The preparation method of inorganic oxide microbeads: Weigh the raw materials of powder precursors (including oxides, carbonates, hydroxides) of each element according to the target ratio, and after ball milling, mixing, pressure filtering, drying, and then High-temperature sintering, coarse crushing, secondary ball milling, and spray drying to obtain fixed-component inorganic oxide microspheres.
无机氧化物微珠，氧化铝，中心粒径D50＝5μm，江苏联瑞新材料股份有限公司，简称氧化铝。Inorganic oxide beads, alumina, center particle size D50=5μm, Jiangsu Lianrui New Material Co., Ltd., alumina for short.
无机氧化物微珠，氧化钙，中心粒径D50＝10μm，简称氧化钙。Inorganic oxide microbeads, calcium oxide, center particle size D50=10μm, referred to as calcium oxide.
无机氧化物微珠，氧化镁，中心粒径D50＝15μm，简称氧化镁。Inorganic oxide beads, magnesium oxide, center particle size D50=15μm, referred to as magnesium oxide.
无机氧化物微珠，二氧化硅，中心粒径D50＝20μm，江苏联瑞新材料股份有限公司，简称二氧化硅。Inorganic oxide beads, silica, center particle size D50=20μm, Jiangsu Lianrui New Material Co., Ltd., silica for short.
有机聚合物微粒——有机硅聚合物微粒：Organic polymer particles-silicone polymer particles:
有机聚合物微粒，KMP-590，有机硅聚合物微粒，平均粒径2μm，信越化学工业株式会社，简称KMP-590。Organic polymer particles, KMP-590, silicone polymer particles, average particle size 2μm, Shin-Etsu Chemical Co., Ltd., KMP-590 for short.
有机聚合物微粒，KMP-597，有机硅聚合物微粒，平均粒径2μm，信越化学工业株式会社，简称KMP-597。Organic polymer particles, KMP-597, silicone polymer particles, with an average particle size of 2μm, Shin-Etsu Chemical Co., Ltd., KMP-597 for short.
有机聚合物微粒，KMP-701，有机硅聚合物微粒，平均粒径3.5μm，信越化学工业株式会社，简称KMP-701。Organic polymer particles, KMP-701, silicone polymer particles, with an average particle size of 3.5 μm, Shin-Etsu Chemical Co., Ltd., KMP-701 for short.
有机聚合物微粒，KMP-600，有机硅聚合物微粒，平均粒径5μm，信越化学工业株式会社，简称KMP-600。Organic polymer particles, KMP-600, silicone polymer particles, average particle size 5μm, Shin-Etsu Chemical Co., Ltd., KMP-600 for short.
有机聚合物微粒，KMP-605，有机硅聚合物微粒，平均粒径2μm，信越化学工业株式会社，简称KMP-605。Organic polymer particles, KMP-605, silicone polymer particles, with an average particle size of 2μm, Shin-Etsu Chemical Co., Ltd., KMP-605 for short.
有机聚合物微粒，X-52-7030，有机硅聚合物微粒，平均粒径0.8μm，信越化学工业株式会社，简称X-52-7030。Organic polymer particles, X-52-7030, silicone polymer particles, average particle size 0.8μm, Shin-Etsu Chemical Co., Ltd., X-52-7030 for short.
有机聚合物微粒，X-52-854，有机硅聚合物微粒，平均粒径0.8μm，信越化学工业株式会社，简称X-52-854。Organic polymer particles, X-52-854, silicone polymer particles, average particle size 0.8μm, Shin-Etsu Chemical Co., Ltd., X-52-854 for short.
有机聚合物微粒——酚醛树脂：Organic polymer particles-phenolic resin:
有机聚合物微粒，酚醛树脂，数均分子量为20000～50000，平均粒径1um，简称酚醛树脂-1。Organic polymer particles, phenolic resin, with a number average molecular weight of 20,000 to 50,000 and an average particle size of 1um, referred to as phenolic resin-1.
有机聚合物微粒，酚醛树脂，数均分子量为30000～80000，平均粒径3um，简称酚醛树脂-2。Organic polymer particles, phenol resin, with a number average molecular weight of 30,000 to 80,000 and an average particle size of 3um, referred to as phenol resin-2.
有机聚合物微粒，酚醛树脂，数均分子量为50000～100000，平均粒径5um，简称酚醛树脂-3。Organic polymer particles, phenolic resin, with a number average molecular weight of 50,000 to 100,000 and an average particle size of 5um, referred to as phenolic resin-3.
有机聚合物微粒——聚苯乙烯微粒：Organic polymer particles-polystyrene particles:
有机聚合物微粒，聚苯乙烯微粒，平均粒径0.5um，简称聚苯乙烯微粒-1。Organic polymer particles, polystyrene particles, with an average particle size of 0.5um, referred to as polystyrene particles-1.
有机聚合物微粒，聚苯乙烯微粒，平均粒径2um，简称聚苯乙烯微粒-2。Organic polymer particles, polystyrene particles, average particle size 2um, referred to as polystyrene particles-2.
有机聚合物微粒，KM-503，聚苯乙烯微粒，平均粒径3μm，东莞市科迈新材料有限公司，简称KM-503。Organic polymer particles, KM-503, polystyrene particles, with an average particle size of 3μm, Dongguan Kemai New Material Co., Ltd., referred to as KM-503.
有机聚合物微粒，KM-5030，聚苯乙烯微粒，平均粒径3μm，东莞市科迈新材料有限公司，简称KM-5030。Organic polymer particles, KM-5030, polystyrene particles, with an average particle size of 3μm, Dongguan Kemai New Material Co., Ltd., referred to as KM-5030.
有机聚合物微粒——聚甲基丙烯酸甲酯微粒：Organic polymer particles-polymethyl methacrylate particles:
有机聚合物微粒，LD-015，聚甲基丙烯酸甲酯微粒，平均粒径1.5μm，东莞市宣成化工科技有限公司。Organic polymer particles, LD-015, polymethyl methacrylate particles, average particle size 1.5μm, Dongguan Xuancheng Chemical Technology Co., Ltd.
有机聚合物微粒，KMR-3EA，聚甲基丙烯酸甲酯微粒，平均粒径3μm，日本综研化学株式会社，简称KER-3EA。Organic polymer particles, KMR-3EA, polymethyl methacrylate particles, with an average particle size of 3μm, Japan Soken Chemical Co., Ltd., referred to as KER-3EA.
有机聚合物微粒，KMR-3TA，聚甲基丙烯酸甲酯微粒，平均粒径3μm，日本综研化学株式会社，简称KMR-3TA。Organic polymer particles, KMR-3TA, polymethyl methacrylate particles, with an average particle size of 3μm, Japan Soken Chemical Co., Ltd., KMR-3TA for short.
黑色素，纳米碳黑2300#，平均粒径15nm，三菱化学株式会社。Melanin, nano carbon black 2300#, average particle size 15nm, Mitsubishi Chemical Corporation.
黑色素，纳米氧化铜，平均粒径40nm，北京德科岛金科技有限公司。Melanin, nano-copper oxide, average particle size 40nm, Beijing Deco Island Gold Technology Co., Ltd.
黑色素，纳米氧化锰，平均粒径50nm，上海比客新材料科技有限公司。Melanin, nano-manganese oxide, average particle size 50nm, Shanghai Bike New Material Technology Co., Ltd.
本发明的实施例是为了使本领域的技术人员能够更好的理解本发明，但并不对本发明作任何限制。The embodiments of the present invention are to enable those skilled in the art to better understand the present invention, but do not impose any limitation on the present invention.
按本发明中实施例和比较例制得的封装树脂组合物将按照以下方法测试其各项性能。The encapsulating resin compositions prepared according to the examples and comparative examples of the present invention will be tested for various properties according to the following methods.
蓝光光衰：将焊有蓝光芯片和导线的六角基板放置在成型设备模具上，然后将制备好的封装树脂组合物经成型设备预热和挤压入模腔，包埋芯片，而裸露六角基板的导线。该样品需在150℃下固化4小时。然后用积分球测试该包埋的芯片在特定电流下点亮时的初始光通量。将一系列需要测试的封装树脂组合物按照该方法制备成待测样品，然后串联在一起，室温下用200mA电流(加速测试)持续点亮200小时，再次测试特定电流下的剩余光通量。(初始光通量-剩余光通量)/初始光通量，即得到该单颗样品的蓝光光衰。每种封装树脂组合物单次测试样品数量不少于3个，取平均值。Blue light decay: Place the hexagonal substrate with blue chip and wire soldered on the mold of the molding equipment, and then preheat and extrude the prepared encapsulating resin composition into the mold cavity through the molding equipment to embed the chip, and expose the hexagonal substrate Wire. The sample needs to be cured at 150°C for 4 hours. Then use the integrating sphere to test the initial luminous flux of the embedded chip when it is lit under a specific current. A series of encapsulating resin compositions to be tested are prepared into samples to be tested according to this method, and then connected in series, lighted continuously with 200mA current (accelerated test) at room temperature for 200 hours, and the remaining luminous flux under a specific current is tested again. (Initial luminous flux-remaining luminous flux)/Initial luminous flux, that is, the blue light attenuation of the single sample is obtained. The number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
该测试中使用的积分球设备是杭州远方光电信息股份有限公司制造的铝基座测光积分球R98.The integrating sphere equipment used in this test is the aluminum base metering integrating sphere R98 manufactured by Hangzhou Yuanfang Optoelectronics Information Co., Ltd.
模塑收缩率：称量制备好的封装树脂组合物粉末或颗粒或块状20g，150℃注塑到特定模具中固化成型。模具型腔为直径60mm的圆形，厚度约3mm。取出固化成型的封装树脂，室温下放置24小时。然后沿垂直方向量取固化树脂的直径，求平均值，得到的直径与模具直径之差，除以模具直径，得到模塑收缩率。每种封装树脂组合物单次测试样品数量不少于3个，取平均值。Molding shrinkage rate: Weigh 20g of the prepared encapsulating resin composition powder or pellets or block, and inject it into a specific mold at 150°C for curing. The mold cavity is a circle with a diameter of 60mm and a thickness of about 3mm. Take out the cured and molded encapsulating resin and place it at room temperature for 24 hours. Then measure the diameter of the cured resin in the vertical direction, calculate the average, and divide the difference between the obtained diameter and the mold diameter by the mold diameter to obtain the mold shrinkage rate. The number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
吸水率：与模塑收缩率制样的模具和注塑条件相同，得到直径60mm，厚度约3mm的样片。在150℃条件下继续固化4小时。取出样片，放置到室温后称量样片质量，为初始重量。然后投入到沸水中持续煮沸1小时，取出样片，擦干水分，称量样片质量。两次质量之差除以初始质量，即为样品的吸水率。每种封装树脂组合物单次测试样品数量不少于3个，取平均值。Water absorption: The mold and injection conditions are the same as the mold shrinkage rate, and the sample with a diameter of 60mm and a thickness of about 3mm is obtained. Continue curing for 4 hours at 150°C. Take out the sample, place it at room temperature, and weigh the sample, which is the initial weight. Then put it into boiling water and continue to boil for 1 hour, take out the sample, wipe off the water, and weigh the quality of the sample. The difference between the two masses divided by the initial mass is the water absorption rate of the sample. The number of test samples for each encapsulation resin composition at a time is not less than 3, and the average value is taken.
出光率：将所得封装树脂组合物挤压进型腔为边长30mm，深度为0.40mm的模具中，150℃固化2分钟，然后再转移到150℃的烘箱中继续固化4小时，制得边长约30mm*30mm，厚度为0.40mm的样片，用分光光度计测试450nm处的光透过率，即为出光率。Light extraction rate: extrude the obtained encapsulating resin composition into a mold with a side length of 30mm and a depth of 0.40mm, cure at 150°C for 2 minutes, and then transfer to an oven at 150°C to continue curing for 4 hours to obtain a side For a sample with a length of about 30mm*30mm and a thickness of 0.40mm, use a spectrophotometer to test the light transmittance at 450nm, which is the light output rate.
出光均匀性：将制备好的封装树脂组合物用注塑成型的方法封装到红光LED芯片上，然后测试该芯片的辐射强度分布数据，即不同角度的辐射强度，判断出光效果。Uniformity of light output: The prepared encapsulating resin composition is encapsulated on a red LED chip by injection molding, and then the radiation intensity distribution data of the chip is tested, that is, the radiation intensity at different angles to determine the light effect.
芯片表面温度：将焊有蓝光芯片和导线的六角基板放置在成型设备模具上，然后将制备好的封装树脂组合物经成型设备预热和挤压入模腔，包埋芯片，包埋厚度为1mm，而裸露六角基板的导线。该样品需在150℃下固化4小时。然后将一系列需要测试的封装树脂组合物按照该方法制备成待测样品，然后串联在一起，室温下用200mA电流(加速测试)持续点亮1小时，用红外热成像仪测试该条件下的芯片表面温度。，即得到该单颗样品的蓝光光衰。每种封装树脂组合物单次测试样品数量不少于3个，取平均值。Chip surface temperature: Place the hexagonal substrate welded with blue light chips and wires on the mold of the molding equipment, and then preheat and extrude the prepared packaging resin composition into the mold cavity through the molding equipment to embed the chip. The embedding thickness is 1mm, and the wires of the hexagonal substrate are exposed. The sample needs to be cured at 150°C for 4 hours. Then a series of encapsulating resin compositions to be tested were prepared into samples to be tested according to this method, and then connected in series, with 200mA current (accelerated test) at room temperature for continuous lighting for 1 hour, and an infrared thermal imager was used to test the samples under this condition Chip surface temperature. , The blue light attenuation of the single sample is obtained. There are no less than 3 samples for each encapsulation resin composition in a single test, and the average value is taken.
红外热成像仪，RX-500，东莞市不凡电子有限公司。Infrared Thermal Imager, RX-500, Dongguan Bufan Electronics Co., Ltd.
本发明中的实施例制备的一种LED显示屏贴片式分立器件用封装树脂组合物(简称封装树脂组合物)：和对比例中封装树脂组合物制备方法如下：An encapsulating resin composition for LED display chip-type discrete devices prepared in the embodiment of the present invention (encapsulating resin composition for short): and the method of preparing the encapsulating resin composition in the comparative example is as follows:
各实施例配比见表1，取第一类环氧树脂(如果有第二类环氧树脂也加上)、酸酐、无机氧化物微珠、有机聚合物微粒和黑色素混合均匀，再使用双螺杆挤出机在100℃下混炼均匀，然后冷却、粉碎后，得到粉末状的封装树脂组合物。The proportion of each example is shown in Table 1. Take the first type epoxy resin (if there is a second type epoxy resin, add it), acid anhydride, inorganic oxide beads, organic polymer particles and melanin and mix them evenly, and then use double The screw extruder is uniformly kneaded at 100°C, then cooled and pulverized to obtain a powdered encapsulating resin composition.
本发明中实施例1～11的测试结果见表2。The test results of Examples 1-11 of the present invention are shown in Table 2.
本发明中比较例，各物质按照表3中所示配比混合，使用双螺杆挤出机在100℃温度下混炼均匀，然后冷却，粉碎后，得到粉末状的封装树脂组合物。In the comparative example of the present invention, the materials were mixed according to the ratio shown in Table 3, mixed uniformly at a temperature of 100° C. using a twin-screw extruder, and then cooled and pulverized to obtain a powdered encapsulating resin composition.
本发明中比较例1～9的测试结果见表3。The test results of Comparative Examples 1-9 in the present invention are shown in Table 3.
根据表1中实施例1～3，7～11结果可知，当环氧树脂的成分全部是第一类环氧树脂时，得到的封装树脂组合物耐蓝光光衰效果显著。According to the results of Examples 1 to 3 and 7 to 11 in Table 1, when all the components of the epoxy resin are the first type epoxy resin, the obtained encapsulating resin composition has a significant effect of resisting blue light and light decay.
在实施例4～6中，将第一类环氧树脂与第二类环氧树脂复合使用时，得到的封装树脂组合物蓝光光衰的表现良好。In Examples 4 to 6, when the first type epoxy resin and the second type epoxy resin are used in combination, the resulting encapsulating resin composition exhibits good blue light attenuation.
用第一类环氧树脂CELLOXIDE 2021P、CELLOXIDE 8000、DGIC或MGIC替换实施例1中的EHPE-3150，可以得到类似的耐蓝光光衰表现。Replacing EHPE-3150 in Example 1 with the first type epoxy resin CELLOXIDE 2021P, CELLOXIDE 8000, DGIC or MGIC can obtain similar blue light resistance performance.
比较例1中，由于全部使用第二类环氧树脂(JER1002)作为主剂，得到的对比例封装树脂组合物对于蓝光光衰的表现差。In Comparative Example 1, since all the second type epoxy resin (JER1002) was used as the main agent, the obtained encapsulating resin composition of the Comparative Example had poor performance against blue light attenuation.
用第二类环氧树脂(包含双酚A型环氧树脂NPES-301、NPES-303、NPES-304、NPES-901、NPES-902、NPES-903、NPES-904、NPES-905、JER1004、JER1007、JER1009、JER1010和JER1003F；氢化双酚A型环氧树脂YX-8000、YX-8040、YX-8034和YL-6753；双酚F型环氧树脂NPEF-170、NPEF-175、NPEF-176、NPEF-185、NPEF-187和NPEF-500；环氧硅胶复合环氧树脂ERS-Si1200、ERS-Si1700和XP833)替换JER1002时，可以得到类似的耐蓝光光衰表现。Use the second type epoxy resin (including bisphenol A epoxy resin NPES-301, NPES-303, NPES-304, NPES-901, NPES-902, NPES-903, NPES-904, NPES-905, JER1004, JER1007, JER1009, JER1010 and JER1003F; hydrogenated bisphenol A epoxy resin YX-8000, YX-8040, YX-8034 and YL-6753; bisphenol F epoxy resin NPEF-170, NPEF-175, NPEF-176 , NPEF-185, NPEF-187 and NPEF-500; epoxy silica gel composite epoxy resin (ERS-Si1200, ERS-Si1700 and XP833) when JER1002 is replaced, similar blue light resistance performance can be obtained.
由实施例1、2和6，以及比较例2和7的结果可知，因封装树脂组合物中含有无机氧化物微珠-1，封装树脂组合物的模塑收缩率和吸水率会明显下降，且无机氧化物 微珠含量增多时，下降程度进一步增加，同时仍具有较高的出光率，保持了相当的透明性，对于发光LED元件意义重大。From the results of Examples 1, 2 and 6, and Comparative Examples 2 and 7, it can be seen that since the encapsulating resin composition contains inorganic oxide beads-1, the molding shrinkage and water absorption of the encapsulating resin composition will be significantly reduced. And when the content of inorganic oxide microbeads increases, the degree of decline further increases, while still having a high light extraction rate and maintaining considerable transparency, which is of great significance to light-emitting LED components.
由实施例2、3、5、9和10可知，因含有无机氧化物微珠-2、无机氧化物微珠-3、无机氧化物微珠-4、无机氧化物微珠-5和无机氧化物微珠-6时，封装树脂组合物的模塑收缩率和吸水率明显下降，且具有较高的出光率，透明性良好。From Examples 2, 3, 5, 9 and 10, it can be seen that due to the inclusion of inorganic oxide beads-2, inorganic oxide beads-3, inorganic oxide beads-4, inorganic oxide beads-5 and inorganic oxide beads When the microbeads-6 are used, the molding shrinkage rate and water absorption rate of the encapsulating resin composition are significantly reduced, and the encapsulation resin composition has a higher light output rate and good transparency.
用无机氧化物微珠-7、无机氧化物微珠-8、无机氧化物微珠-9、无机氧化物微珠-10、无机氧化物微珠-11或无机氧化物微珠-12代替实施例1中的无机氧化物微珠-1时，可以得到类似的效果。Use inorganic oxide beads-7, inorganic oxide beads-8, inorganic oxide beads-9, inorganic oxide beads-10, inorganic oxide beads-11 or inorganic oxide beads-12 instead of implementation In the case of inorganic oxide beads-1 in Example 1, a similar effect can be obtained.
比较例2中，由于未添加无机氧化物微珠，得到的封装树脂组合物模塑收缩率较高，吸水率表现也较差。In Comparative Example 2, since no inorganic oxide beads were added, the molding shrinkage rate of the obtained encapsulating resin composition was high, and the water absorption performance was also poor.
比较例3中，由于使用了普通的无机氧化物微珠二氧化硅，虽然得到的封装树脂组合物模塑收缩率和吸水率也有明显下降，但其出光率非常低，对于发光元件来说失去了添加的意义，更不适用于RGB显示屏的应用。In Comparative Example 3, due to the use of ordinary inorganic oxide microbead silica, although the molding shrinkage rate and water absorption rate of the obtained encapsulating resin composition are also significantly reduced, the light extraction rate is very low, which is lost for light-emitting elements. In addition to the added meaning, it is not suitable for RGB display applications.
通过比较例1和比较例7，可以发现，在未使用有机聚合物微粒的情况下，封装树脂组合物仍具有一定的均匀出光效果。因此本发明所使用的无机氧化物微珠还起到一定均衡各角度出光的作用。Through Comparative Example 1 and Comparative Example 7, it can be found that the encapsulating resin composition still has a certain uniform light emitting effect without using organic polymer particles. Therefore, the inorganic oxide microbeads used in the present invention also have a certain balance of light emission from various angles.
由实施例1、2、7和8可知，因含有有机聚合物微粒KMP-590时，封装树脂组合物的出光曲线形状为光滑弧型，说明各角度出光均匀，有机聚合物微粒KMP-590起到了均衡各角度出光的作用。From Examples 1, 2, 7 and 8, it can be seen that when organic polymer particles KMP-590 are contained, the light emission curve shape of the encapsulating resin composition is a smooth arc shape, indicating that the light is uniform at all angles, and the organic polymer particles KMP-590 start To balance the role of light from all angles.
由实施例3～5可知，添加有机聚合物微粒酚醛树脂-1，KM-503和KMR-3EA，得到的封装树脂组合物，出光曲线同样为光滑弧形。说明有机聚合物微粒酚醛树脂-1，KM-503和KMR-3EA同样具有均衡各角度出光的作用。It can be seen from Examples 3 to 5 that the encapsulation resin composition obtained by adding organic polymer microparticle phenol resin-1, KM-503 and KMR-3EA has a smooth arc shape. It shows that the organic polymer microparticle phenolic resin-1, KM-503 and KMR-3EA also have the effect of balancing light emission from various angles.
通过比较例7可知，未添加有机聚合物微粒的封装树脂组合物，测得各角度出光强度差异大，曲线形状呈锯齿状，不能各角度均匀出光。It can be seen from Comparative Example 7 that the encapsulating resin composition without adding organic polymer particles has a large difference in light intensity measured at various angles, the curve shape is zigzag, and the light cannot be emitted uniformly at each angle.
用有机聚合物微粒KMP-597、KMP-701、KMP-600、KMP-605、X-52-7030、X-52-854、酚醛树脂-2、酚醛树脂-3、聚苯乙烯微粒-1、聚苯乙烯微粒-2、KM-5030、LD-015和KMR-3TA替代实施例1中的有机聚合物微粒KMP-590时，得到的封装树脂组合物出光曲线可以达到类似的效果。Organic polymer particles KMP-597, KMP-701, KMP-600, KMP-605, X-52-7030, X-52-854, phenolic resin-2, phenolic resin-3, polystyrene particles-1, When polystyrene particles-2, KM-5030, LD-015 and KMR-3TA replace the organic polymer particles KMP-590 in Example 1, the light emission curve of the obtained encapsulating resin composition can achieve a similar effect.
同时，通过实施例2、实施例7和实施例8可知，含有有机聚合物微粒KMP-590较多时会明显提高封装树脂组合物的吸水率，加大可靠性失效的风险。因此有机聚合物微粒不能单独使用，需要复合无机氧化物微珠，消除因吸水率升高带来的风险。At the same time, it can be known from Example 2, Example 7 and Example 8 that when there are more organic polymer particles KMP-590, the water absorption rate of the encapsulating resin composition is significantly increased, and the risk of reliability failure is increased. Therefore, organic polymer particles cannot be used alone, and composite inorganic oxide beads are required to eliminate the risk of increased water absorption.
实施例1～11中分别使用了黑色素纳米级碳黑2300#(平均粒径15nm)和黑色素纳米级氧化铜(平均粒径40nm)，起到了提高对比度的效果，同时保证出光率和较低的芯片表面温度。In Examples 1 to 11, melanin nanometer carbon black 2300# (average particle size 15nm) and melanin nanometer copper oxide (average particle size 40nm) were used respectively to improve the contrast, while ensuring the light output rate and lower Chip surface temperature.
在比较例9中，过多添加黑色素纳米碳黑2300#，一方面导致出光率下降严重，另一方面黑色素吸热导致热量积聚在封装好的元件内，长期点亮后引起温度升高，增加了经久使用的LED器件失效的风险。In Comparative Example 9, excessive addition of melanin nano-carbon black 2300#, on the one hand, caused a serious drop in light output, on the other hand, the heat absorption of melanin caused heat to accumulate in the packaged component, which caused the temperature to increase after long-term lighting. This reduces the risk of failure of LED devices that have been used for a long time.
用纳米氧化锰(平均粒径50nm)替代实施例1黑色素纳米碳黑2300#(平均粒径15nm)可以得到类似的效果。Substituting nano-manganese oxide (average particle size 50nm) for Example 1 melanin nano-carbon black 2300# (average particle size 15nm) can obtain a similar effect.
用偏苯三甲酸酐、均苯四甲酸二酐、氢化均苯四甲酸二酐、甲基四氢苯二甲酸酐、纳迪克酸酐、十二烯基丁二酸酐、甲基纳迪克酸酐、氢化甲基纳迪克酸酐、戊二酸酐、甲基环己烯四羧酸二酐替代实施例1中的顺丁烯二酸酐时，可以得到类似的效果。Use trimellitic anhydride, pyromellitic dianhydride, hydrogenated pyromellitic dianhydride, methyltetrahydrophthalic anhydride, nadic anhydride, dodecenyl succinic anhydride, methyl nadic anhydride, hydrogenated methane When kinadic anhydride, glutaric anhydride, and methylcyclohexenetetracarboxylic dianhydride are substituted for maleic anhydride in Example 1, similar effects can be obtained.
由以上结果可知，本发明的一种LED显示屏贴片式分立器件用封装树脂组合物具有耐蓝光光衰，吸水率低的特点，增加了小型化、薄型化器件气密保护性和可靠性。同时该环氧树脂组合物的模塑收缩率得到了降低，有效抑制小间距高密度芯片封装后的翘曲，改善了封装厂的操作性问题。It can be seen from the above results that the encapsulating resin composition for LED display chip discrete devices of the present invention has the characteristics of blue light decay resistance, low water absorption, and increases the airtight protection and reliability of miniaturized and thin devices. . At the same time, the molding shrinkage rate of the epoxy resin composition is reduced, and the warpage after the small-pitch high-density chip packaging is effectively suppressed, and the operability problem of the packaging factory is improved.
从应用体验方面，本发明中封装树脂组合物通过平衡R、G、B芯片各角度出光强度，使得封装完成的芯片组屏且正面调白平衡后，大角度随视角而产生的颜色偏差消失。精细化添加适当黑色素在不引起芯片温度升高的同时还可以提高对比度。From the aspect of application experience, the encapsulating resin composition of the present invention balances the light intensity of the R, G, and B chips at various angles, so that after the packaged chip set screen is white and balanced on the front side, the color deviation caused by the large angle with the viewing angle disappears. The refined addition of appropriate melanin can improve the contrast without causing the chip temperature to rise.
表3table 3
注：Note:
1)Ⅰ类：光滑弧形，各角度出光强度均匀。1) Type I: Smooth arc, uniform light intensity at all angles.
2)Ⅱ类：锯齿状，各角度出光强度差异巨大。2) Class Ⅱ: Zigzag, with huge difference in light intensity from various angles.
3)Ⅲ类：中心角度有微小凹陷的弧形，中心角度出光强度略低。3) Type III: arc shape with a slight depression in the center angle, and the light intensity at the center angle is slightly lower.
4)*：由于出光率低，无法测得蓝光光衰和出光曲线形状。4)*: Due to the low light output rate, the blue light decay and light curve shape cannot be measured.
5)表1和表3中，括号里的数字表示环氧树脂或酸酐的摩尔数。5) In Table 1 and Table 3, the numbers in parentheses indicate the number of moles of epoxy resin or acid anhydride.
本发明筛选出第一类和第二类环氧树脂体系，加入酸酐，并进一步引入无机氧化物微珠。考虑到发光元件的光透过率，本发明使用筛选的无机氧化物微珠，具有较高的透过率。且无机氧化物微珠的含量占第一类环氧树脂、第二类环氧树脂和无机氧化 物微珠的5～60份。由于无机氧化物微珠的导热系数普遍大于环氧树脂，因此一定程度上还提升了该组合物的散热效果。The present invention screens out the first and second types of epoxy resin systems, adds acid anhydride, and further introduces inorganic oxide microspheres. Considering the light transmittance of the light-emitting element, the present invention uses selected inorganic oxide microbeads, which have a higher transmittance. And the content of the inorganic oxide microbeads accounts for 5-60 parts of the first type epoxy resin, the second type epoxy resin and the inorganic oxide microbeads. Since the thermal conductivity of inorganic oxide microbeads is generally greater than that of epoxy resin, the heat dissipation effect of the composition is also improved to a certain extent.
为了进一步增强光型的配光效果(出光均匀性)，本发明提出在加入无机氧化物微珠的同时复配有机聚合物微粒，该有机聚合物微粒可以起到混合R、G、B三种芯片发出光的作用，能够在大角度平衡显示各角度的出光。对于组装完的大尺寸显示屏，正面调白平衡后侧面大角度观察无红光。In order to further enhance the light distribution effect (light uniformity) of the light type, the present invention proposes to add organic polymer particles while adding inorganic oxide beads. The organic polymer particles can mix R, G, and B. The light emitted by the chip can balance the light emitted from various angles at a large angle. For the assembled large-size display, there is no red light when viewed from the side at a large angle after the front white balance is adjusted.
本发明提出添加黑色素来达到提高对比度的目的，但鉴于黑色素吸收热量导致发光元件温度升高，且黑色素添加量多时发光元件的透光性急剧下降的特点，黑色素的用量严格限制在0.1％重量以下。The present invention proposes to add melanin to achieve the purpose of improving contrast. However, in view of the characteristics that the temperature of the light-emitting element rises due to the absorption of heat by melanin, and the light transmittance of the light-emitting element decreases sharply when the amount of melanin is added, the amount of melanin is strictly limited to 0.1% by weight or less .
从而获得一种具有低光衰，抗翘曲，耐潮气的封装树脂组合物，还能够平衡出光、提高对比度和散热性，提升终端用户体验。Thus, an encapsulating resin composition with low light attenuation, warpage resistance, and moisture resistance is obtained, which can also balance light output, improve contrast and heat dissipation, and enhance end user experience.
本发明封装的LED器件，封装层厚度一般在0.2～0.6mm。The thickness of the packaging layer of the LED device packaged in the present invention is generally 0.2-0.6 mm.

Claims (1)

  1. 一种LED显示屏贴片式分立器件用封装树脂组合物，其特征是包括第一类环氧树脂、第二类环氧树脂、酸酐、无机氧化物微珠、有机聚合物微粒和黑色素。2.根据权利要求1所述的组合物，其特征是所述第一类环氧树脂的质量为10～61份，第二类环氧树脂的质量为0～60份，酸酐用量与第一类环氧树脂和第二类环氧树脂的环氧基团为等摩尔比，无机氧化物微珠的质量为5～60份，有机聚合物微粒的质量为第一类环氧树脂、第二类环氧树脂、酸酐和无机氧化物微珠总质量的0.1％-1％；黑色素的质量为第一类环氧树脂、第二类环氧树脂、酸酐和无机氧化物微珠总质量的0.01％～0.1％。3.根据权利要求1或2所述的组合物，其特征是所述第一类环氧树脂为脂环族环氧树脂、异氰尿酸缩水甘油酯中的至少一种；所述脂环族环氧树脂为聚[(2-环氧乙烷基)-1,2-环己二醇]2-乙基-2-(羟甲基)-1,3-丙二醇醚、3,4-环氧环己基甲基3,4-环氧环己基甲酸酯或大赛璐CELLOXIDE 8000。所述异氰尿酸缩水甘油酯为异氰尿酸三缩水甘油酯、异氰尿酸二缩水甘油酯或异氰尿酸单缩水甘油酯。4.根据权利要求1或2所述的组合物，其特征是所述第二类环氧树脂为双酚A型环氧树脂、氢化双酚A型环氧树脂、双酚F型环氧树脂或环氧硅胶复合环氧树脂。5.根据权利要求1或2所述的组合物，其特征是所述酸酐为四氢苯二甲酸酐、苯二甲酸酐、偏苯三甲酸酐、均苯四甲酸二酐、氢化均苯四甲酸二酐、顺丁烯二酸酐、甲基四氢苯二甲酸酐、六氢苯二甲酸酐、甲基六氢苯二甲酸酐、纳迪克酸酐、十二烯基丁二酸酐、甲基纳迪克酸酐、氢化甲基纳迪克酸酐、戊二酸酐、甲基环己烯四羧酸二酐中至少一种。6.根据权利要求1或2所述的组合物，其特征是所述无机氧化物微珠的通式为Na(1-x-y-z-u)O(1-x-y-z-u)/2·SixO2x·M1yO3y/2·M2zOz·ZruO2u，其中M1＝B、Al；M2＝Mg、Ca、Sr、Zn。对各元素的含量，0.4≤x≤0.7；0.1≤y≤0.3；z≤0.3；u≤0.3；x+y+z+u≥0.9，其中z、u与1-x-y-z-u不能同时为零，所述无机氧化物微珠的中心粒径为5～30μm。7.根据权利要求1或2所述的组合物，其特征是所述有机聚合物微粒为有机硅聚合物微粒酚醛树脂微粒、聚苯乙烯微粒和聚甲基丙烯酸甲酯微粒中至少一种，所述有机聚合物微粒平均粒径在5μm以下。8.根据权利要求1或2所述的组合物，其特征是所述黑色素为纳米炭黑、纳米氧化铜和纳米氧化锰中至少一种。9.权利要求1-8之一所述组合物在LED显示屏贴片式RGB分立器件封装的应用。An encapsulation resin composition for LED display screen patch type discrete devices, which is characterized by comprising a first type epoxy resin, a second type epoxy resin, acid anhydride, inorganic oxide beads, organic polymer particles and melanin. 2. The composition according to claim 1, wherein the mass of the first type epoxy resin is 10 to 61 parts, the mass of the second type epoxy resin is 0 to 60 parts, and the amount of acid anhydride is the same as that of the first type epoxy resin. The epoxy groups of the epoxy resin and the second epoxy resin are in an equimolar ratio, the mass of the inorganic oxide beads is 5-60 parts, and the mass of the organic polymer particles is the first epoxy resin and the second epoxy resin. 0.1%-1% of the total mass of epoxy resin, acid anhydride and inorganic oxide microbeads; the mass of melanin is 0.01 of the total mass of the first epoxy resin, second epoxy resin, acid anhydride and inorganic oxide microbeads %～0.1%. 3. The composition according to claim 1 or 2, wherein the first type of epoxy resin is at least one of alicyclic epoxy resin and glycidyl isocyanurate; The epoxy resin is poly[(2-oxiranyl)-1,2-cyclohexanediol] 2-ethyl-2-(hydroxymethyl)-1,3-propanediol ether, 3,4-ring Oxycyclohexyl methyl 3,4-epoxycyclohexyl formate or CELLOXIDE 8000. The glycidyl isocyanurate is triglycidyl isocyanurate, diglycidyl isocyanurate or monoglycidyl isocyanurate. 4. The composition according to claim 1 or 2, wherein the second type of epoxy resin is bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, and bisphenol F epoxy resin. Or epoxy silicone composite epoxy resin. 5. The composition according to claim 1 or 2, wherein the acid anhydride is tetrahydrophthalic anhydride, phthalic anhydride, trimellitic anhydride, pyromellitic dianhydride, hydrogenated pyromellitic anhydride Dianhydride, maleic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, Nadic anhydride, dodecenyl succinic anhydride, methyl Nadic At least one of acid anhydride, hydrogenated methyl nadic acid anhydride, glutaric acid anhydride, and methylcyclohexene tetracarboxylic dianhydride. 6. The composition according to claim 1 or 2, characterized in that the general formula of the inorganic oxide beads is Na(1-xyzu)O(1-xyzu)/2·SixO2x·M1yO3y/2·M2zOz · ZruO2u, where M1=B, Al; M2=Mg, Ca, Sr, Zn. For the content of each element, 0.4≤x≤0.7; 0.1≤y≤0.3; z≤0.3; u≤0.3; x+y+z+u≥0.9, where z, u and 1-xyzu cannot be zero at the same time, so The central particle size of the inorganic oxide beads is 5-30 μm. 7. The composition according to claim 1 or 2, wherein the organic polymer particles are at least one of silicone polymer particles, phenol resin particles, polystyrene particles and polymethyl methacrylate particles, The average particle size of the organic polymer particles is less than 5 μm. 8. The composition according to claim 1 or 2, wherein the melanin is at least one of nano carbon black, nano copper oxide and nano manganese oxide. 9. The application of the composition according to any one of claims 1 to 8 in the packaging of LED display chip RGB discrete devices.
PCT/CN2020/072357 2019-05-30 2020-01-16 Encapsulating resin composition for led display screen smt discrete device and application thereof WO2020238261A1 (en)

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