Potting material and preparation method thereof, potting glue and electronic product

Abstract

The present application discloses a potting material and a preparation method thereof, a potting glue and an electronic product. The potting material includes the following raw materials by mass percentage: 2% to 12% of liquid bisphenol A epoxy resin, 0.5% to 12% of liquid bisphenol F epoxy resin, 2% to 12% of alicyclic epoxy resin, 0.1% to 10% of toughening resin, 0.1% to 10% of active diluent, 5% to 20% of curing agent and 65% to 85% of auxiliary agent; wherein the curing agent includes a modified curing agent, and the modified curing agent includes an addition product of a basic anhydride and a basic alcohol. The above-mentioned potting material has high toughness and glass transition temperature, which makes it heat-resistant and deformation-resistant, not easy to crack, and avoids warping problems. At the same time, the shrinkage rate and thermal expansion coefficient of the above-mentioned potting material are low, and it has good reliability.

Description

Technical Field

[0001] The present application relates to the field of organic materials, and in particular to a potting material and a preparation method thereof, a potting glue and an electronic product. Background Art

[0002] With the development of various consumer digital products, semiconductors are increasingly moving towards lightness, thinness, small size and high performance. Liquid potting materials are developed to follow this development trend. The four-sided pinless flat package is a surface mount package that retracts the output pins originally around the package body to the bottom of the package body, thereby greatly reducing the space occupied during the patch operation. This package structure is particularly suitable for application environments that have requirements for size, weight and performance due to its small size and light weight, as well as its outstanding electrical and thermal properties.

[0003] Traditional materials suitable for liquid encapsulation have poor mechanical properties and heat resistance, and often suffer from problems such as warping. Summary of the invention

[0004] Based on this, in order to improve the heat resistance and mechanical properties of the potting material, it is necessary to provide a potting material and a preparation method thereof, a potting glue and an electronic product.

[0005] The present application provides a potting material, which includes the following raw materials by mass percentage:

[0006] Liquid bisphenol A epoxy resin 2%~12%,

[0007] Liquid bisphenol F epoxy resin 0.5%~12%,

[0008] Alicyclic epoxy resin 2%~12%,

[0009] Toughening resin 0.1%~10%,

[0010] Active diluent 0.1%~10%,

[0011] Curing agent 5%~20%, and

[0012] Additives 65%~85%;

[0013] Wherein, the curing agent includes a modified curing agent, the modified curing agent includes an esterification product of a basic acid anhydride and a basic alcohol, the basic acid anhydride includes one or more of trimellitic anhydride, pyromellitic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, 3,3,4,4-diphenyl sulfone tetracarboxylic dianhydride, 9,9-bis(3,4-dicarboxyphenyl)fluorene dianhydride and 4,4'-(4,4'-isopropyldiphenoxy) diphthalic anhydride, and the viscosity of the basic alcohol is 1 cp~500cp.

[0014] In one embodiment, the preparation method of the modified curing agent comprises the following steps:

[0015] The base anhydride and the base alcohol are mixed, heated to 80° C. to 180° C. in an inert gas, and reacted for 1 h to 18 h.

[0016] In one embodiment, the base anhydride and the base alcohol are mixed in a molar ratio of (1-5): 1. In one embodiment, one or more of the following conditions are met:

[0017] (1) The epoxy equivalent of the liquid bisphenol A epoxy resin is 170 g / eq to 250 g / eq;

[0018] (2) The viscosity of the liquid bisphenol A epoxy resin is 3000 cp ~ 50000 cp;

[0019] (3) The epoxy equivalent of the liquid bisphenol F epoxy resin is 150 g / eq to 220 g / eq;

[0020] (4) The viscosity of the liquid bisphenol F epoxy resin is 1500 cp ~ 13000 cp;

[0021] (5) The epoxy equivalent of the alicyclic epoxy resin is 100 g / eq to 200 g / eq;

[0022] (6) The viscosity of the alicyclic epoxy resin is 100cp~3500cp;

[0023] (7) The toughening resin comprises a toughening agent and an epoxy resin prepolymer in a mass ratio of (0.8-1.3):1, wherein the toughening agent comprises one or more of nitrile rubber, polyurethane elastomer, silicone elastomer and polyacrylate elastomer;

[0024] (8) The active diluent includes one or both of a monofunctional active diluent and a multifunctional active diluent;

[0025] The monofunctional reactive diluent includes one or more of C8-C10 alkyl glycidyl ether, C12-C14 alkyl glycidyl ether, cardanol glycidyl ether, butyl glycidyl ether, benzyl alcohol glycidyl ether and o-cresol glycidyl ether;

[0026] The multifunctional active diluent includes one or more of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycerol triglycidyl ether, neopentyl glycol diglycidyl ether, trimethylolpropane triglycidyl ether and polyethylene glycol glycidyl ether.

[0027] In one embodiment, the auxiliary agent is calculated by weight, and its raw material composition includes 1 to 5 parts of a curing accelerator, 500 to 900 parts of an inorganic filler, 5 to 15 parts of a silane coupling agent, 0.5 to 5 parts of a defoaming agent, 0.5 to 5 parts of a dispersant, 0.5 to 8 parts of a thixotropic agent, and 0.5 to 3 parts of a colorant.

[0028] In one embodiment, the following raw materials are included by weight percentage:

[0029] Liquid bisphenol A epoxy resin 2%~10%,

[0030] Liquid bisphenol F epoxy resin 0.5%~8%,

[0031] Alicyclic epoxy resin 2%~10%,

[0032] Toughening resin 0.1%~5%,

[0033] Active diluent 0.1%~5%,

[0034] Curing agent 8%~15%,

[0035] Curing accelerator 0.1%~0.8%,

[0036] Inorganic filler 70%~80%,

[0037] Silane coupling agent 0.5%~8%,

[0038] Defoaming agent 0.01%~5%,

[0039] Dispersant 0.01%~5%,

[0040] Thixotropic agent 0.01%~5%, and

[0041] Colorant 0.01%~5%.

[0042] In one embodiment, the auxiliary agent satisfies one or more of the following conditions:

[0043] (1) The curing accelerator includes an imidazole curing accelerator;

[0044] (2) The particle size D50 of the inorganic filler is 0.5 μm to 40 μm;

[0045] (3) The inorganic filler includes silicon dioxide.

[0046] Furthermore, the present application provides a method for preparing a potting material, comprising the following steps:

[0047] Prepare the raw materials of the potting material as described above;

[0048] The liquid bisphenol A epoxy resin, the liquid bisphenol F epoxy resin, the alicyclic epoxy resin, the toughening resin, the reactive diluent, the curing agent and the auxiliary agent are mixed and stirred.

[0049] The present application also provides a potting adhesive, including the potting material as described above.

[0050] Furthermore, the present application also provides an electronic product, which includes a packaging structure, and the packaging structure includes the above-mentioned potting material or the above-mentioned potting glue.

[0051] This application uses liquid bisphenol A epoxy resin, liquid bisphenol F epoxy resin, alicyclic epoxy resin and toughening resin as base resin, and uses addition products of base anhydride and base alcohol as modified curing agent. Under the action of active diluent and auxiliary agent, the toughness and glass transition temperature of the potting material are effectively improved, making it heat-resistant and deformation-resistant, not easy to crack, and avoiding warping problems. At the same time, the shrinkage rate and thermal expansion coefficient of the above-mentioned potting material are low, and it has good reliability. DETAILED DESCRIPTION

[0052] The present application can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thoroughly understood. Of course, they are only examples, and the purpose is not to limit the present application. In addition, the present application can repeat reference numbers and / or letters in different examples. This repetition is for the purpose of simplification and clarity, and does not itself indicate the relationship between the various embodiments and / or settings discussed.

[0053] The words "preferably", "more preferably" and the like in this application refer to embodiments of the present application that may provide certain beneficial effects in certain circumstances. However, other embodiments may also be preferred under the same circumstances or in other circumstances. In addition, the statement of one or more preferred embodiments does not imply that other embodiments are not available, nor is it intended to exclude other embodiments from the scope of this application.

[0054] When a numerical range is disclosed herein, the above range is considered to be continuous and includes the minimum and maximum values ​​of the range, as well as every value between such minimum and maximum values. Further, when a range refers to an integer, every integer between the minimum and maximum values ​​of the range is included. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be combined. In other words, unless otherwise indicated, all ranges disclosed herein should be understood to include any and all subranges included therein.

[0055] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0056] The present application provides a potting material, which includes the following raw materials by mass percentage:

[0057] Liquid bisphenol A epoxy resin 2%~12%,

[0058] Liquid bisphenol F epoxy resin 0.5%~12%,

[0059] Alicyclic epoxy resin 2%~12%,

[0060] Toughening resin 0.1%~10%,

[0061] Active diluent 0.1%~10%,

[0062] Curing agent 5%~20%, and

[0063] Additives 65%~85%;

[0064] The curing agent includes a modified curing agent, the modified curing agent includes an addition product of a basic acid anhydride and a basic alcohol, the basic acid anhydride includes one or more of trimellitic anhydride (TMA), pyromellitic dianhydride (PMDA), 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA), 3,3,4,4-diphenylsulfonetetracarboxylic dianhydride (DSDA), 9,9-bis(3,4-dicarboxyphenyl)fluorene dianhydride (BPAF) and 4,4'-(4,4'-isopropyldiphenoxy)phthalic anhydride, and the viscosity of the basic alcohol is 1cp~500cp.

[0065] Specifically, the viscosity of the base alcohol at 25° C. is 1 cp to 500 cp. Specifically, the viscosity of the base alcohol at 25° C. may be, but is not limited to, 1 cp, 10 cp, 11 cp, 12 cp, 13 cp, 14 cp, 15 cp, 16 cp, 17 cp, 18 cp, 19 cp, 20 cp, 50 cp, 75 cp, 100 cp, 125 cp, 150 cp, 175 cp, 200 cp, 225 cp, 250 cp, 275 cp, 300 cp, 325 cp, 350 cp, 375 cp, 400 cp, 425 cp, 450 cp, 475 cp or 500 cp. Preferably, the base alcohol comprises benzyl alcohol, and the viscosity of benzyl alcohol at 25° C. is 13 cp.

[0066] Furthermore, the curing agent also includes anhydride curing agents, and specifically the anhydride curing agent may be, but is not limited to, one or more of methyl hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, methyl nadic anhydride and hydrogenated methyl nadic anhydride.

[0067] Furthermore, the curing agent is a modified curing agent, or the curing agent can also be a modified curing agent and an acid anhydride curing agent in a mass ratio of 1: (0.8~2.2).

[0068] In a specific example, the preparation method of the modified curing agent includes the following steps:

[0069] Mix the base anhydride and the base alcohol, heat to 80℃~180℃ in an inert gas, and react for 1 h~18h.

[0070] Specifically, a base anhydride and a base alcohol are mixed in a molar ratio of (1-5):1, and the base anhydride and the base alcohol can be mixed in a molar ratio of but not limited to 1:1, 2:1, 3:1, 4:1 or 5:1, and a solvent propylene glycol methyl ether acetate (PGMEA) is added to a reactor, and the air is replaced by nitrogen, and heating is performed until the reaction is completed.

[0071] Further, the heating temperature may be, but is not limited to, 80° C., 90° C., 100° C., 110° C., 120° C., 130° C., 140° C., 150° C., 160° C., 170° C., or 180° C. The reaction time may be, but is not limited to, 1 h, 2 h, 3 h, 4 h, 5 h, 6 h, 7 h, 8 h, 9 h, 10 h, 11 h, 12 h, 13 h, 14 h, 15 h, 16 h, 17 h, or 18 h.

[0072] It can be understood that after the reaction is completed, it also includes atmospheric distillation until no liquid drips out, connecting a vacuum pump to vacuum distillation until no liquid drips out, determining that the reaction is completed, and discharging. Specifically, the temperature of atmospheric distillation and the temperature of vacuum distillation are each independently 100°C to 160°C, and the temperature of atmospheric distillation and the temperature of vacuum distillation can be independently but not limited to 100°C, 110°C, 120°C, 130°C, 140°C, 150°C or 160°C.

[0073] In a specific example, the liquid bisphenol A epoxy resin satisfies one or both of the following conditions:

[0074] (1) Epoxy equivalent is 170g / eq~250g / eq;

[0075] (2) Viscosity is 3000 cp ~50000cp.

[0076] It can be understood that epoxy equivalent refers to the molar number of epoxy functional groups contained in a unit mass of epoxy resin. It is usually expressed as: Ep = W / Me

[0077] Wherein, Ep is the epoxy equivalent, W is the molecular weight of the epoxy resin, and Me is the molecular weight of the epoxy functional group.

[0078] Specifically, the epoxy equivalent of the liquid bisphenol A epoxy resin can be, but is not limited to, 170 g / eq, 180 g / eq, 190 g / eq, 200 g / eq, 210 g / eq, 220 g / eq, 230 g / eq, 240 g / eq or 250 g / eq.

[0079] The viscosity of the liquid bisphenol A type epoxy resin at 25° C. may be, but is not limited to, 3000 cp, 5000 cp, 7000 cp, 9000 cp, 11000 cp, 12000 cp, 13000 cp, 14000 cp, 15000 cp, 16000 cp, 18000 cp, 20000 cp, 22000 cp, 24000 cp, 26000 cp, 28000 cp, 30000 cp, 32000 cp, 34000 cp, 36000 cp, 38000 cp, 40000 cp, 42000 cp, 44000 cp, 46000 cp, 48000 cp or 50000 cp.

[0080] In a specific example, the liquid bisphenol F epoxy resin satisfies one or both of the following conditions:

[0081] (1) Epoxy equivalent is 150g / eq~220g / eq;

[0082] (2) Viscosity is 1500 cp ~13000 cp.

[0083] Specifically, the epoxy equivalent of the liquid bisphenol F epoxy resin may be, but is not limited to, 150 g / eq, 160 g / eq, 170 g / eq, 180 g / eq, 190 g / eq, 200 g / eq, 210 g / eq or 220 g / eq. The viscosity of the liquid bisphenol F type epoxy resin at 25° C. may be, but is not limited to, 1500 cp, 1700 cp, 1900 cp, 2100 cp, 2300 cp, 2500 cp, 2700 cp, 2900 cp, 3100 cp, 3300 cp, 3500 cp, 3600 cp, 3700 cp, 3800 cp, 3900 cp, 4000 cp, 4200 cp, 4400 cp, 4600 cp, 4800 cp, 5000 cp, 5200 cp, 5400 cp, 5600 cp, 5800 cp, 6000 cp, 6200 cp, 6400 cp, 6600 cp, 6800 cp, 7000 cp, 7200 cp, 7300 cp, 7400 cp, 7500 cp, 7600 cp, 7700 cp, 7800 cp, 7900 cp, 8000 cp, 8100 cp, 8200 cp, 8300 cp, 8400 cp cp, 7400 cp, 7600 cp, 7800 cp, 8000cp, 8200 cp, 400 cp, 8600 cp, 8800 cp, 9000 cp, 9200 cp, 9400 cp, 9600 cp, 9800 cp, 10000 cp, 10500 cp, 11000 cp, 11500 cp, 12000 cp, 12500 cp or 13000cp.

[0084] In a specific example, the cycloaliphatic epoxy resin satisfies one or both of the following conditions:

[0085] (1) Epoxy equivalent is 100g / eq~200g / eq;

[0086] (2) Viscosity: 100cp~3500cp.

[0087] Specifically, the epoxy equivalent of the alicyclic epoxy resin may be, but is not limited to, 100 g / eq, 110 g / eq, 120 g / eq, 130 g / eq, 140 g / eq, 150 g / eq, 160 g / eq, 170 g / eq, 180 g / eq, 190 g / eq, or 200 g / eq. The viscosity of the alicyclic epoxy resin at 25° C. may be, but is not limited to, 100 cp, 120 cp, 140 cp, 160 cp, 200 cp, 240 cp, 280 cp, 320 cp, 340 cp, 360 cp, 380 cp, 400 cp, 420 cp, 440 cp, 460 cp, 480 cp, 500 cp, 600 cp, 700 cp, 800 cp, 900 cp, 1000 cp, 1100 cp, 120 0cp, 1300cp, 1400cp, 1500cp, 1600cp, 1700cp, 1800cp, 1900cp, 2000cp, 2100cp, 2200cp, 2300cp, 2400cp, 2500cp, 2600cp, 2700cp, 2800cp, 2900cp, 3000cp, 3100cp, 3200cp, 3300cp, 3400cp or 3500cp.

[0088] In a specific example, the additive is calculated by weight, and its raw material composition includes 1 to 5 parts of a curing accelerator, 500 to 900 parts of an inorganic filler, 5 to 15 parts of a silane coupling agent, 0.5 to 5 parts of a defoaming agent, 0.5 to 5 parts of a dispersant, 0.5 to 8 parts of a thixotropic agent, and 0.5 to 3 parts of a colorant.

[0089] In a specific example, the following raw materials are included in mass percentage:

[0090] Liquid bisphenol A epoxy resin 2%~10%,

[0091] Liquid bisphenol F epoxy resin 0.5%~8%,

[0092] Alicyclic epoxy resin 2%~10%,

[0093] Toughening resin 0.1%~5%,

[0094] Active diluent 0.1%~5%,

[0095] Curing agent 8%~15%,

[0096] Curing accelerator 0.1%~0.8%,

[0097] Inorganic filler 70%~80%,

[0098] Silane coupling agent 0.5%~8%,

[0099] Defoaming agent 0.01%~5%,

[0100] Dispersant 0.01%~5%,

[0101] Thixotropic agent 0.01%~5%, and

[0102] Colorant 0.01%~5%.

[0103] Preferably, the following raw materials are included in percentage by mass:

[0104] Liquid bisphenol A epoxy resin 2%~8%,

[0105] Liquid bisphenol F epoxy resin 0.5%~5%,

[0106] Alicyclic epoxy resin 2%~8%,

[0107] Toughening resin 0.1%~2%,

[0108] Active diluent 0.1%~2%,

[0109] Curing agent 8%~13%,

[0110] Curing accelerator 0.1%~0.5%,

[0111] Inorganic filler 70%~78%,

[0112] Silane coupling agent 0.5%~5%,

[0113] Defoaming agent 0.01%~1%,

[0114] Dispersant 0.01%~1%,

[0115] Thixotropic agent 0.01%~1%, and

[0116] Colorant 0.01%~1%.

[0117] In a specific example, the curing accelerator includes an imidazole curing accelerator. Specifically, the imidazole accelerator includes one or more of PN50, PN23 and PNH.

[0118] Furthermore, the defoaming agent includes an organosilicon defoaming agent, the dispersant includes a titanium dispersant, and the thixotropic agent includes a hydrophobic fumed silica thixotropic agent.

[0119] In a specific example, the particle size D50 of the inorganic filler is 0.5 μm to 40 μm.

[0120] Further, the particle sizes D50 of the inorganic fillers each independently include 0.5 μm to 1.0 μm, 1.5 μm to 2.0 μm, 3 μm to 5 μm, 15 μm to 18 μm, and 25 μm to 40 μm.

[0121] In one specific example, the inorganic filler includes silica.

[0122] Preferably, the inorganic filler is spherical silica.

[0123] It can be understood that the inorganic filler includes spherical silica with a particle size D50 of 0.5μm~1.0μm, spherical silica with a particle size D50 of 1.5μm~2.0μm, spherical silica with a particle size D50 of 3μm~5μm, spherical silica with a particle size D50 of 15μm~18μm and spherical silica with a particle size D50 of 25μm~40μm.

[0124] In a specific example, the toughening resin includes a toughening agent modified epoxy resin, and the toughening agent includes one or more of nitrile rubber, polyurethane elastomer, silicone elastomer and polyacrylate elastomer. It can be understood that the toughening resin reacts with the epoxy resin first to increase compatibility and achieve a better toughening effect. The epoxy resin can be, but is not limited to, a liquid bisphenol A epoxy resin or a liquid bisphenol F epoxy resin.

[0125] Specifically, the toughening resin is a prepolymer of a toughening agent and an epoxy resin in a mass ratio of (0.8-1.3):1, and the reaction conditions of the toughening agent and the epoxy resin include: reacting at 90° C.-140° C. for 4 h-8 h under nitrogen protection.

[0126] Further, the toughening resin may be, but is not limited to, a prepolymer of a toughening agent and an epoxy resin in a mass ratio of 0.8:1, 0.85:1, 0.9:1, 0.95:1, 1:1, 1.05:1, 1.1:1, 1.15:1, 1.2:1, 1.25:1 or 1.3:1.

[0127] In a specific example, the reactive diluent includes one or two of a monofunctional reactive diluent and a multifunctional reactive diluent, the monofunctional reactive diluent includes one or more of C8-C10 alcohol glycidyl ether, C12-C14 alcohol glycidyl ether, cardanol glycidyl ether, butyl glycidyl ether, benzyl alcohol glycidyl ether and o-cresol glycidyl ether, and the multifunctional reactive diluent includes one or more of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycerol triglycidyl ether, neopentyl glycol diglycidyl ether, trimethylolpropane triglycidyl ether and polyethylene glycol glycidyl ether.

[0128] Furthermore, the present application provides a method for preparing a potting material, comprising the following steps:

[0129] Prepare the raw materials of the potting material as described above;

[0130] Liquid bisphenol A epoxy resin, liquid bisphenol F epoxy resin, alicyclic epoxy resin, toughening resin, reactive diluent, curing agent and auxiliary agent are mixed and stirred.

[0131] In terms of mass percentage, liquid bisphenol A epoxy resin, liquid bisphenol F epoxy resin, alicyclic epoxy resin, toughening resin, reactive diluent and curing agent are mixed and stirred for the first time, then inorganic filler is added and stirred for the second time, then silane coupling agent, defoamer, dispersant, thixotropic agent and colorant are added and stirred for the third time, and finally curing accelerator is added and stirred for the fourth time.

[0132] Optionally, the temperature of each stirring is independently 5°C to 30°C. Specifically, the temperature of each stirring can be, but is not limited to, 5°C, 15°C, 20°C, 25°C, or 30°C.

[0133] Optionally, the stirring rates of each time independently include a revolution speed of 1000 r / min to 3000 r / min and a rotation ratio of 30% to 60%. Specifically, the revolution speed of each stirring can be but not limited to 1000r / min, 1100r / min, 1200r / min, 1300r / min, 1400r / min, 1500r / min, 1600r / min, 1700r / min, 1800r / min, 1900r / min, 2000r / min, 2100r / min, 2200r / min, 2300r / min, 2400r / min, 2500r / min, 2600r / min, 2700r / min, 2800r / min, 2900r / min or 3000r / min, and the rotation ratio of each stirring can be but not limited to 30%, 35%, 40%, 45%, 50%, 55% or 60%.

[0134] Optionally, the stirring time for each time independently includes 1 min to 5 min, and the stirring time for each time can be but is not limited to 1 min, 2 min, 3 min, 4 min or 5 min.

[0135] The present application also provides a potting adhesive, including the potting material as described above.

[0136] Furthermore, the present application also provides an electronic product, the electronic product includes a packaging structure, the packaging structure includes the above-mentioned potting material or the above-mentioned potting glue.

[0137] This application uses liquid bisphenol A epoxy resin, liquid bisphenol F epoxy resin, alicyclic epoxy resin and toughening resin as base resin, and uses addition products of base anhydride and base alcohol as modified curing agent. Under the action of active diluent and auxiliary agent, the toughness and glass transition temperature of the potting material are effectively improved, making it heat-resistant and deformation-resistant, not easy to crack, and avoiding warping problems. At the same time, the shrinkage rate and thermal expansion coefficient of the above-mentioned potting material are low, and it has good reliability.

[0138] The following specific examples are provided to further illustrate the potting material and preparation method of the present application in detail. Unless otherwise specified, the raw materials involved in the following specific implementation methods can all be sourced from commercial sources.

[0139] Among them, 830 is bisphenol F epoxy resin, which comes from Nantong Xingchen Synthetic Materials Co., Ltd., with an epoxy equivalent of 160g / eq and a viscosity of 3873cp at 25°C. The equivalent and viscosity of the corresponding grades are different

[0140] BE188EL is a bisphenol A epoxy resin sourced from the Changchun Artificial Resin Factory in Taiwan, China. Its epoxy equivalent is 185 g / eq and its viscosity at 25°C is 13873 cp.

[0141] S-21 is an alicyclic epoxy resin sourced from Nantong Synasia New Materials Co., Ltd. It has an epoxy equivalent of 137 g / eq and a viscosity of 140.80 cp at 25°C.

[0142] Monofunctional active diluent, from Nantong Xingchen Synthetic Materials Co., Ltd., model 3630, the main component is C12-C14 alkyl glycidyl ether; 3692, the main component is benzyl alcohol glycidyl ether; 3660, the main component is butyl glycidyl ether.

[0143] Multifunctional active diluent, from Nantong Xingchen Synthetic Materials Co., Ltd., model 3622, 1,4-butanediol diglycidyl ether; 3636, propylene glycol triglycidyl ether, trimethylolpropane triglycidyl ether, model V36, from Nantong Xingchen Synthetic Materials Co., Ltd., epoxy equivalent is 150g / eq, viscosity at 25°C is 137cp. The equivalent and viscosity corresponding to the brand are different.

[0144] MNA stands for methylnadic anhydride, which is an anhydride curing agent and comes from Jining Tangyi Chemical Co., Ltd.

[0145] MTHPA stands for methyltetrahydrophthalic anhydride, which is an anhydride curing agent and comes from Jining Tangyi Chemical Co., Ltd.

[0146] MHHPA stands for methyl hexahydrophthalic anhydride, which is an anhydride curing agent and comes from Jining Tangyi Chemical Co., Ltd.

[0147] A-1 (TMA-BA) is a modified curing agent, which is self-prepared. Trimellitic anhydride (TMA) comes from Adamas Reagent Co., Ltd., and benzyl alcohol comes from Shanghai Aladdin Biochemical Technology Co., Ltd.

[0148] A-2 (PMDA-BA) is a modified curing agent, which is self-prepared. PMDA comes from Adamas Reagent Co., Ltd., and benzyl alcohol comes from Shanghai Aladdin Biochemical Technology Co., Ltd.

[0149] PN23 is an imidazole curing accelerator, which comes from Japan Ajinomoto Fine Technology Co., Ltd.

[0150] M0420 is spherical SiO2 with a particle size D50 of 3.78 μm, sourced from Zhejiang Huafei Electronic Substrate Co., Ltd.

[0151] NQ105 is spherical SiO2 with a particle size D50 of 15 μm, sourced from Jiangsu Lianrui New Materials Co., Ltd.

[0152] KH560 is a silane coupling agent from Shanghai Titan Technology Co., Ltd.

[0153] BYK-A530 is a defoaming agent from BYK Chemicals.

[0154] KYC-918 is a dispersant from Keying Chemical.

[0155] R-106 is a thixotropic agent, which comes from Evonik Degussa.

[0156] CB is carbon black, a colorant, derived from Orion.

[0157] Preparation method of modified curing agent A-1:

[0158] 0.2 mol of trimellitic anhydride (TMA), 0.1 mol of benzyl alcohol and 100 g of propylene glycol methyl ether acetate (PGMEA) were added into the reactor, the air was replaced by nitrogen, the mixture was heated to 100°C and reacted for 2 hours; then, it was distilled at 130°C under normal pressure until no liquid dripped out, and then it was connected to a vacuum pump and distilled at 130°C under reduced pressure until no liquid dripped out, the reaction was determined to be complete, and the product was discharged and recorded as A-1 (TMA-BA).

[0159] Preparation method of modified curing agent A-2:

[0160] 0.2 mol of pyromellitic dianhydride (PMDA), 0.1 mol of benzyl alcohol and 100 g of propylene glycol methyl ether acetate (PGMEA) were added into the reactor, the air was replaced by nitrogen, the mixture was heated to 110°C and reacted for 5 hours; then, it was distilled at 150°C under normal pressure until no liquid dripped out, and then it was connected to a vacuum pump and distilled at 150°C under reduced pressure until no liquid dripped out, the reaction was determined to be complete, and the product was discharged, which was recorded as A-2 (PMDA-BA).

[0161] Example 1

[0162] This embodiment provides a liquid encapsulation material and a preparation method thereof, the steps are as follows:

[0163] Please refer to Table 1. In terms of mass percentage, 5.73wt% of 188EL, 1.15wt% of 830, 4.58wt% of S-21, 0.57wt% of CTBN and 188EL were reacted at a mass ratio of 1.15:1 at 90℃~140℃ for 4h~8h under nitrogen protection to obtain a prepolymer, 0.57wt% of active diluent (trimethylolpropane triglycidyl ether) and 5.72wt% of MHHPA, 5.73wt% of A-2 (PMDA-BA) were mixed, and stirred in a non-invasive homogenizer at a revolution speed of 2500r / min and a rotation ratio of 35% for 5min, followed by adding 57.27wt% of NQ105 and 17.18wt% M0420 was added and stirred for 3 min at an orbital speed of 2500 r / min and a rotation ratio of 35%, and then 1.03wt% of KH560, 0.06wt% of BYK-A530, 0.07wt% of KYC-918, 0.11wt% of R-106 and 0.06wt% of CB were added and stirred for 2 min at an orbital speed of 2500 r / min and a rotation ratio of 35%, and finally 0.17wt% of PN-23 was added and stirred for 2 min at an orbital speed of 2500 r / min and a rotation ratio of 35%, and vacuum degassing and stirring were performed at an orbital speed of 1200 r / min and a rotation ratio of 35% for 5 min to obtain a liquid potting material.

[0164] The obtained liquid encapsulating material was subjected to the following performance tests at room temperature, and the results are summarized in Table 1:

[0165] 1) Initial viscosity at 25℃: measured by a rotational viscometer in accordance with GB / T 2794, unit: Pa.s;

[0166] 2) Flexural modulus: measured by dynamic thermomechanical analyzer, unit: MPa;

[0167] 3) Glass transition temperature (Tg): measured by dynamic thermomechanical analyzer;

[0168] 4) Tensile strength: tested by universal testing machine, unit is MPa;

[0169] 5) Elongation at break: tested using a universal testing machine, the unit is %.

[0170] 6) Thermal expansion coefficient: measured by static thermomechanical analyzer (TMA), unit is ppm.

[0171] 7) Shrinkage rate: measured by precision electronic balance, unit is %

[0172] The raw material selection and specific proportions of other embodiments and comparative examples are shown in Table 1. According to the liquid encapsulation material preparation method of Example 1, the liquid encapsulation materials of Examples 2 to 5 and the liquid encapsulation materials of Comparative Examples 1 to 3 are prepared.

[0173] The properties of the liquid encapsulating materials obtained in Examples 2 to 5 and Comparative Examples 1 to 3 were tested in the same manner as in Example 1 and are summarized in Table 1.

[0174] Table 1

[0175]

[0176] “ / ” means that the substance is not added.

[0177] The properties of the liquid encapsulating materials obtained in Examples 2 to 5 and Comparative Examples 1 to 3 were tested in the same manner as in Example 1 and are summarized in Table 2.

[0178] Table 2

[0179]

[0180] It can be seen from Tables 1 and 2 that the mechanical properties and glass transition temperature of the potting material using the modified curing agent are greatly improved, making the modified material resistant to heat and deformation, not easy to crack, and avoiding the warping problem in the package. At the same time, the shrinkage rate and thermal expansion coefficient of the above potting material are low, and it has good reliability.

[0181] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0182] The above-described embodiments only express several implementation methods of the present application, which is convenient for understanding the technical solution of the present application in detail, but it cannot be understood as limiting the scope of protection of the invention patent. It should be pointed out that for ordinary technicians in this field, without departing from the concept of the present application, several variations and improvements can be made, which all belong to the protection scope of the present application. It should be understood that the technical solutions obtained by those skilled in the art through logical analysis, reasoning or limited experiments on the basis of the technical solutions provided in the present application are all within the protection scope of the claims attached to the present application. Therefore, the scope of protection of the patent of this application shall be based on the content of the attached claims, and the description can be used to interpret the content of the claims.

Claims

1. A potting material, characterized in that: The following raw materials are included in percentage by mass: Wherein, the curing agent includes a modified curing agent, and the modified curing agent includes an esterification product of a basic acid anhydride and a basic alcohol in a molar ratio of (1 to 5):1, the basic acid anhydride includes one or more of trimellitic anhydride, pyromellitic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, 3,3,4,4-diphenyl sulfone tetracarboxylic dianhydride, 9,9-bis(3,4-dicarboxyphenyl)fluorene dianhydride and 4,4'-(4,4'-isopropyldiphenoxy) diphthalic anhydride, and the basic alcohol is benzyl alcohol.

2. The potting material according to claim 1, characterized in that: The preparation method of the modified curing agent comprises the following steps: The base anhydride and the base alcohol are mixed, heated to 80° C. to 180° C. in an inert gas, and reacted for 1 h to 18 h.

3. The potting material according to claim 1, characterized in that: The active diluent includes one or two of a monofunctional active diluent and a multifunctional active diluent; The monofunctional reactive diluent includes one or more of C8-C10 alkyl glycidyl ether, C12-C14 alkyl glycidyl ether, cardanol glycidyl ether, butyl glycidyl ether, benzyl alcohol glycidyl ether and o-cresol glycidyl ether; The multifunctional active diluent includes one or more of 1,4-butanediol diglycidyl ether, 1,6-hexanediol diglycidyl ether, glycerol triglycidyl ether, neopentyl glycol diglycidyl ether, trimethylolpropane triglycidyl ether and polyethylene glycol glycidyl ether.

4. The potting material according to claim 1, characterized in that: One or more of the following conditions are met: (1) The epoxy equivalent of the liquid bisphenol A epoxy resin is 170 g / eq to 250 g / eq; (2) The viscosity of the liquid bisphenol A epoxy resin is 3000cp to 50000cp; (3) The epoxy equivalent of the liquid bisphenol F epoxy resin is 150 g / eq to 220 g / eq; (4) The viscosity of the liquid bisphenol F epoxy resin is 1500cp to 13000cp; (5) The epoxy equivalent of the alicyclic epoxy resin is 100 g / eq to 200 g / eq; (6) The viscosity of the alicyclic epoxy resin is 100 cp to 3500 cp; (7) The toughening resin includes a toughening agent and an epoxy resin prepolymer in a mass ratio of (0.8 to 1.3):1, and the toughening agent includes one or more of nitrile rubber, polyurethane elastomer, silicone elastomer and polyacrylate elastomer.

5. The potting material according to any one of claims 1 to 4, characterized in that: The auxiliary agent is calculated by weight, and its raw material composition includes 1 to 5 parts of curing accelerator, 500 to 900 parts of inorganic filler, 5 to 15 parts of silane coupling agent, 0.5 to 5 parts of defoamer, 0.5 to 5 parts of dispersant, 0.5 to 8 parts of thixotropic agent and 0.5 to 3 parts of colorant.

6. The potting material according to claim 5, characterized in that: The following raw materials are included in percentage by mass:

7. The potting material according to claim 5, characterized in that: The auxiliary agent meets one or more of the following conditions: (1) The curing accelerator includes an imidazole curing accelerator; (2) The particle size D50 of the inorganic filler is 0.5 μm to 40 μm; (3) The inorganic filler includes silicon dioxide.

8. A method for preparing a potting material, characterized in that: The following steps are involved: Preparation of raw materials for the potting material according to any one of claims 1 to 7; The liquid bisphenol A epoxy resin, the liquid bisphenol F epoxy resin, the alicyclic epoxy resin, the toughening resin, the reactive diluent, the curing agent and the auxiliary agent are mixed and stirred.

9. A potting glue, characterized in that: The invention comprises the potting material as claimed in any one of claims 1 to 7.

10. An electronic product, characterized in that: The electronic product comprises a packaging structure, and the packaging structure comprises the potting material according to any one of claims 1 to 7 or the potting glue according to claim 9.

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