Epoxy resin plastic packaging material and preparation method and application thereof

Abstract

The application relates to the technical field of semiconductor packaging, and discloses an epoxy resin plastic packaging material, a preparation method and application thereof, the method comprises the following steps: (1) mixing epoxy resin, phenolic resin, a curing accelerator, inorganic fillers, a release agent, a modified silane coupling agent and optional flame retardants, optional colorants and optional modifiers to obtain a mixture, and then melt-kneading the mixture; (2) carrying out back-temperature treatment on the material obtained in the step (1); the modified silane coupling agent comprises a hydrolytic silane coupling agent and optional silane coupling agents. The epoxy resin plastic packaging material prepared by the method has necessary fluidity and bonding performance, and has a good application prospect in the field of semiconductor packaging.

Description

Technical Field

[0001] This invention relates to the field of semiconductor packaging technology, specifically to an epoxy resin encapsulation material, its preparation method, and its application. Background Technology

[0002] With the continuous development of semiconductor devices, increasingly higher requirements are being placed on semiconductor packaging technology and product performance. Among these, product appearance is the most fundamental influencing factor. The appearance defects of a product can promote and accelerate the failure of semiconductor packaged devices. The more surface pores a semiconductor device has, the greater its impact on the product. Solving the problem of surface pores requires a multi-pronged approach, addressing issues from the perspectives of packaging design, packaging process parameters, and packaging materials. Therefore, reducing the number of surface pores can significantly improve product performance. Summary of the Invention

[0003] The purpose of this invention is to overcome the problem of premature failure of semiconductor packaging devices in the prior art, and to provide an epoxy resin encapsulation material. This epoxy resin encapsulation material has the necessary flowability and adhesion properties. When applied in the field of semiconductor packaging, the encapsulated semiconductor device has low surface porosity and good performance.

[0004] To achieve the above objectives, the present invention provides a method for preparing epoxy resin molding compound, the method comprising the following steps:

[0005] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, mold release agent and modified silane coupling agent, as well as optional flame retardant, optional colorant and optional modifier are mixed to obtain a mixture, and then the mixture is melt-kneaded.

[0006] (2) The material obtained in step (1) is subjected to a reheating process;

[0007] The modified silane coupling agent includes a hydrolyzed silane coupling agent and an optional silane coupling agent.

[0008] Preferably, the mixture comprises 6-19% by weight of epoxy resin, 3-9% by weight of phenolic resin, 0.1-0.5% by weight of curing accelerator, 70-87% by weight of inorganic filler, 0.2-1% by weight of release agent, 0.2-0.8% by weight of modified silane coupling agent, 0-8% by weight of flame retardant, 0-1% by weight of colorant and 0-1% by weight of modifier, with the total weight of the mixture being 100%.

[0009] Preferably, the preparation method of the hydrolyzed silane coupling agent is as follows: the silane coupling agent and water are mixed and then reacted.

[0010] Preferably, the weight ratio of silane coupling agent to water is 2 to 5:1.

[0011] Preferably, the reaction conditions include a temperature of 25–55°C and a time of 0.5–4 h.

[0012] Preferably, when the modified silane coupling agent is a hydrolyzed silane coupling agent and a silane coupling agent, the weight ratio of the hydrolyzed silane coupling agent to the silane coupling agent is 0.5 to 3:1.

[0013] Preferably, the silane coupling agent is selected from one or more of γ-glycidoxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-aminopropyltrimethoxysilane, methyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, and N-phenyl-3-aminopropyltrimethoxysilane.

[0014] Preferably, the epoxy resin is selected from one or more of the following: o-cresol epoxy resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin, polyphenolic glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, alicyclic epoxy resin, and heterocyclic epoxy resin.

[0015] Preferably, the phenolic resin is selected from one or more of the following: linear phenolic resin and its derivatives, linear phenolic resin and its derivatives, monohydroxy or dihydroxynaphthol phenolic resin and its derivatives, condensates of p-xylene and phenol, condensates of p-xylene and naphthol, and copolymers of dicyclopentadiene and phenol.

[0016] Preferably, the curing accelerator is selected from one or more of 2-methylimidazole, 2,4-dimethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-butylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, triphenylphosphine, 1,8-diazabicycloundec-7-ene, and triphenylphosphine-1,4-benzoquinone.

[0017] Preferably, the inorganic filler is selected from one or more of alumina, titanium dioxide, silicon nitride, aluminum nitride, and silicon dioxide.

[0018] Preferably, the release agent is selected from one or more of carnauba wax, synthetic wax, and paraffin wax.

[0019] Preferably, the flame retardant is selected from one or more of halogenated flame retardants, phosphorus-based flame retardants, nitrogen-based flame retardants, phosphorus-halogenated flame retardants, phosphorus-nitrogenated flame retardants, and hydroxide flame retardants.

[0020] Preferably, the colorant is selected from one or more of titanium dioxide, zinc oxide, zinc barium white and carbon black.

[0021] Preferably, the modifier is liquid silicone oil and / or silicone rubber.

[0022] A second aspect of the present invention provides an epoxy resin encapsulating material prepared by the above method.

[0023] A third aspect of the present invention provides the application of the above-mentioned epoxy resin encapsulation material in the field of semiconductor packaging.

[0024] Compared with existing technologies, the technical solution of this invention has the following advantages: the epoxy resin encapsulating material possesses the necessary fluidity and adhesion. This may be because, under high-temperature conditions, the hydrolyzed silane coupling agent more readily reacts with the hydroxyl groups on the surface of the inorganic filler described in this invention, thereby increasing the mixing uniformity of the epoxy resin encapsulating material during processing. Simultaneously, after temperature recovery treatment, the epoxy resin and phenolic resin undergo slight cross-linking under the action of a curing accelerator, optimizing the fluidity of the epoxy resin encapsulating material. When this epoxy resin encapsulating material is used to encapsulate semiconductor devices, venting is easier during the encapsulation process, thus reducing the formation of pores and resulting in encapsulated semiconductor devices with very low surface porosity. Detailed Implementation

[0025] The following provides a detailed description of specific embodiments of the present invention. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.

[0026] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0027] The first aspect of this invention provides a method for preparing epoxy resin molding compound, the method comprising the following steps:

[0028] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, mold release agent and modified silane coupling agent, as well as optional flame retardant, optional colorant and optional modifier are mixed to obtain a mixture, and then the mixture is melt-kneaded.

[0029] (2) The material obtained in step (1) is subjected to a reheating process;

[0030] The modified silane coupling agent includes a hydrolyzed silane coupling agent and an optional silane coupling agent.

[0031] In this invention, the raw material silane coupling agent used in the hydrolytic silane coupling agent and the optional silane coupling agent can be the same or different.

[0032] In a preferred embodiment, the total weight of the mixture is 100%, and the mixture contains 6-19% by weight of epoxy resin, 3-9% by weight of phenolic resin, 0.1-0.5% by weight of curing accelerator, 70-87% by weight of inorganic filler, 0.2-1% by weight of release agent, 0.2-0.8% by weight of modified silane coupling agent, 0-8% by weight of flame retardant, 0-1% by weight of colorant and 0-1% by weight of modifier.

[0033] In specific embodiments, the epoxy resin content can be 6 wt%, 7 wt%, 8 wt%, 8.5 wt%, 9 wt%, 10 wt%, 11 wt%, 13 wt%, 15 wt%, 17 wt%, or 19 wt%.

[0034] In specific embodiments, the content of phenolic resin can be 3% by weight, 3.5% by weight, 4% by weight, 5% by weight, 6% by weight, 7% by weight, 8% by weight, or 9% by weight.

[0035] In specific embodiments, the content of the curing accelerator can be 0.1% by weight, 0.2% by weight, 0.3% by weight, 0.4% by weight, or 0.5% by weight.

[0036] In specific embodiments, the content of inorganic filler can be 70 wt%, 71 wt%, 72 wt%, 73 wt%, 74 wt%, 75 wt%, 76 wt%, 77 wt%, 78 wt%, 79 wt%, 80 wt%, 85 wt%, or 87 wt%.

[0037] In specific embodiments, the content of the release agent can be 0.2% by weight, 0.3% by weight, 0.4% by weight, 0.5% by weight, 0.6% by weight, 0.7% by weight, 0.8% by weight, 0.9% by weight, or 1% by weight.

[0038] In specific embodiments, the content of the modified silane coupling agent can be 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, or 0.8 wt%.

[0039] In specific embodiments, the flame retardant content can be 2% by weight, 3% by weight, 4% by weight, 5% by weight, 6% by weight, 7% by weight, or 8% by weight.

[0040] In a preferred embodiment, the preparation method of the hydrolyzed silane coupling agent is as follows: the silane coupling agent and water are mixed and then reacted.

[0041] In a preferred embodiment, in order to make the hydrolysis of the silane coupling agent more complete, the weight ratio of the silane coupling agent to water is 2 to 5:1.

[0042] In a preferred embodiment, to further promote the hydrolysis of the silane coupling agent, the reaction conditions include: a temperature of 25–55°C and a time of 0.5–4 h.

[0043] In a specific embodiment, a silane coupling agent and water are mixed to obtain a mixed solution, and the reaction is carried out under stirring until the mixed solution becomes colorless and transparent.

[0044] In a preferred embodiment, when the modified silane coupling agent is a hydrolyzed silane coupling agent and a silane coupling agent, the weight ratio of the hydrolyzed silane coupling agent to the silane coupling agent is 0.5 to 3:1; specifically, the weight ratio of the hydrolyzed silane coupling agent to the silane coupling agent can be 0.5:1, 0.6:1, 1:1, 1.5:1, 1.7:1, 2:1, 2.5:1, 2.8:1, or 3:1.

[0045] In a preferred embodiment, in step (1), melt mixing is carried out in an open rubber mixing mill, and the conditions for melt mixing include: temperature of 75-110°C and time of 6-15 min.

[0046] In a specific implementation, step (1) also includes post-processing such as cooling, crushing and patting the melt-blended material.

[0047] In a preferred embodiment, the conditions for the rewarming treatment in step (2) include: a temperature of 30 to 40°C and a time of 10 to 20 hours.

[0048] In a preferred embodiment, the silane coupling agent is selected from one or more of γ-glycidoxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-aminopropyltrimethoxysilane, methyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, and N-phenyl-3-aminopropyltrimethoxysilane.

[0049] In a preferred embodiment, the epoxy resin is selected from one or more of the following: o-cresol epoxy resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin, polyphenolic glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, alicyclic epoxy resin, and heterocyclic epoxy resin.

[0050] In a preferred embodiment, the phenolic resin is selected from one or more of the following: linear phenolic resin and its derivatives, linear phenolic resin and its derivatives, monohydroxy or dihydroxynaphthol phenolic resin and its derivatives, condensates of p-xylene and phenol, condensates of p-xylene and naphthol, and copolymers of dicyclopentadiene and phenol.

[0051] In a preferred embodiment, the curing accelerator is selected from one or more of 2-methylimidazole, 2,4-dimethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-butylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, triphenylphosphine, 1,8-diazabicycloundec-7-ene, and triphenylphosphine-1,4-benzoquinone.

[0052] In a preferred embodiment, the inorganic filler is selected from one or more of alumina, titanium dioxide, silicon nitride, aluminum nitride, and silicon dioxide.

[0053] In this invention, the inorganic filler is used in a micro powder state with a size of 2 to 200 μm.

[0054] In a preferred embodiment, the release agent is selected from one or more of carnauba wax, synthetic wax, and paraffin wax.

[0055] In a preferred embodiment, the flame retardant is selected from one or more of halogenated flame retardants, phosphorus-based flame retardants, nitrogen-based flame retardants, phosphorus-halogenated flame retardants, phosphorus-nitrogenated flame retardants, and hydroxide flame retardants.

[0056] In a specific embodiment, the flame retardant is zinc borate.

[0057] In a preferred embodiment, the colorant is selected from one or more of titanium dioxide, zinc oxide, zinc barium white, and carbon black.

[0058] In a preferred embodiment, the modifier is liquid silicone oil and / or silicone rubber.

[0059] A second aspect of the present invention provides an epoxy resin encapsulating material prepared by the above method.

[0060] The epoxy resin encapsulating material prepared by the above method possesses the necessary flowability and adhesion. This may be because, under high-temperature conditions, the hydrolyzed silane coupling agent more readily reacts with the hydroxyl groups on the surface of the inorganic filler described in this invention, thereby increasing the mixing uniformity of the epoxy resin encapsulating material during processing. Simultaneously, after temperature recovery treatment, the epoxy resin and phenolic resin undergo slight cross-linking under the action of the curing accelerator, optimizing the flowability of the epoxy resin encapsulating material, facilitating venting during encapsulation, and thus reducing the formation of pores.

[0061] A third aspect of the present invention provides the application of the above-mentioned epoxy resin encapsulation material in the field of semiconductor packaging.

[0062] When semiconductor devices are encapsulated using the aforementioned epoxy resin encapsulation material, the good fluidity of the epoxy resin makes it easier to release air during the encapsulation process. This results in lower surface porosity for the semiconductor devices encapsulated using this epoxy resin encapsulation material, leading to better performance of the encapsulated semiconductor devices.

[0063] The following examples further illustrate the epoxy resin encapsulation material, its preparation method, and its application according to the present invention. These examples are implemented based on the technical solution of the present invention, providing detailed implementation methods and specific operating procedures; however, the scope of protection of the present invention is not limited to the following examples.

[0064] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods in the art. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available.

[0065] Table 1

[0066]

[0067] Example 1

[0068] The raw materials for preparing epoxy resin molding compound S1 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerator is 2-phenyl-4-methylimidazole; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0069] Preparation of hydrolyzed silane coupling agent M1:

[0070] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the reaction was carried out under stirring at a temperature of 30°C for 1 hour until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M1.

[0071] Modified silane coupling agent K1 is the same as hydrolyzed silane coupling agent M1;

[0072] Preparation of epoxy resin molding compound S1:

[0073] (1) Mix epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K1, flame retardant, colorant and modifier, and then melt-mix in an open rubber mixing mill at a temperature of 85°C for 7 minutes. Cool, crush and cake the melt-mixed material.

[0074] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 35°C for 15 hours.

[0075] Example 2

[0076] The raw materials for preparing epoxy resin molding compound S2 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerators are 2-phenyl-4-methylimidazole and 2-undecylimidazole, wherein the weight ratio of 2-phenyl-4-methylimidazole to 2-undecylimidazole is 16:23; the inorganic filler is silica; the silane coupling agent is γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0077] Preparation of hydrolyzed silane coupling agent M2:

[0078] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the mixture was stirred and reacted at 30°C for 2.5 hours until the mixed solution was colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M2.

[0079] Modified silane coupling agent K2 is the same as hydrolyzed silane coupling agent M2;

[0080] Preparation of epoxy resin molding compound S2:

[0081] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K2, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 85°C for 8 minutes. The melt-mixed material is cooled, crushed and caked.

[0082] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 30°C for 20 hours.

[0083] Example 3

[0084] The raw materials for preparing epoxy resin molding compound S3 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerator is 2-ethyl-4-methylimidazolium; the inorganic filler is silica; the silane coupling agent is γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0085] Preparation of hydrolyzed silane coupling agent M3:

[0086] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the mixture was stirred and reacted at a temperature of 30°C for 2 hours until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M3.

[0087] Modified silane coupling agent K3 is composed of hydrolyzed silane coupling agent M3 and silane coupling agent, wherein the weight ratio of hydrolyzed silane coupling agent M3 to silane coupling agent is 59:21.

[0088] Preparation of epoxy resin molding compound S3:

[0089] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K3, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 90°C for 6 minutes. The melt-mixed material is cooled, crushed and caked.

[0090] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 35°C for 15 hours.

[0091] Example 4

[0092] The raw materials for preparing epoxy resin molding compound S4 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerator is 2-undecylimidazole; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0093] Preparation of hydrolyzed silane coupling agent M4:

[0094] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the reaction was carried out under stirring at a temperature of 35°C for 2 hours until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M4.

[0095] Modified silane coupling agent K4 is a combination of hydrolyzed silane coupling agent M4 and silane coupling agent, wherein the weight ratio of hydrolyzed silane coupling agent M4 to silane coupling agent is 3:1.

[0096] Preparation of epoxy resin molding compound S4:

[0097] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K4, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 100°C for 10 minutes. The melt-mixed material is then cooled, crushed and caked.

[0098] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 30°C for 20 hours.

[0099] Example 5

[0100] The raw materials for preparing epoxy resin molding compound S5 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerator is 2-undecylimidazole; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0101] Preparation of hydrolyzed silane coupling agent M5:

[0102] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the reaction was carried out under stirring at a temperature of 35°C for 2 hours until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M5.

[0103] Modified silane coupling agent K5 is the same as hydrolyzed silane coupling agent M5;

[0104] Preparation of epoxy resin molding compound S5:

[0105] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K5, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 75°C for 15 minutes. The melt-mixed material is then cooled, crushed and caked.

[0106] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 35°C for 15 hours.

[0107] Example 6

[0108] The raw materials for preparing epoxy resin molding compound S6 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerators are 2-phenyl-4-methylimidazole and 2-ethyl-4-methylimidazole, wherein the weight ratio of 2-phenyl-4-methylimidazole to 2-ethyl-4-methylimidazole is 7:3; the inorganic filler is silica; the silane coupling agent is γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0109] Preparation of hydrolyzed silane coupling agent M6:

[0110] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the mixture was stirred and reacted at a temperature of 40°C for 1 hour until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M6.

[0111] Modified silane coupling agent K6 is composed of hydrolyzed silane coupling agent M6 and silane coupling agent, wherein the weight ratio of hydrolyzed silane coupling agent M6 to silane coupling agent is 1:1.

[0112] Preparation of epoxy resin molding compound S6:

[0113] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K6, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 80°C for 12 minutes. The melt-mixed material is then cooled, crushed and caked.

[0114] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 35°C for 15 hours.

[0115] Example 7

[0116] The raw materials for preparing epoxy resin molding compound S7 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerators are 2-phenyl-4-methylimidazole and 2-undecylimidazole, wherein the weight ratio of 2-phenyl-4-methylimidazole to 2-undecylimidazole is 3:2; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane and γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0117] Preparation of hydrolyzed silane coupling agent M7:

[0118] The silane coupling agent and water were mixed in a weight ratio of 3:1, and then the mixture was stirred and reacted at a temperature of 40°C for 2 hours until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M7.

[0119] Modified silane coupling agent K7 is the same as hydrolyzed silane coupling agent M7, wherein the weight ratio of hydrolyzed γ-aminopropyltriethoxysilane and hydrolyzed γ-mercaptopropyltrimethoxysilane is 5:3.

[0120] Preparation of epoxy resin molding compound S7:

[0121] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K7, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 110°C for 6 minutes. The melt-mixed material is then cooled, crushed and caked.

[0122] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 30°C for 20 hours.

[0123] Example 8

[0124] The raw materials for preparing epoxy resin molding compound S8 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerators are 2-phenyl-4-methylimidazole, 2-undecylimidazole and 2-ethyl-4-methylimidazole, wherein the weight ratio of 2-phenyl-4-methylimidazole, 2-undecylimidazole and 2-ethyl-4-methylimidazole is 10:21:13; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane and γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0125] Preparation of hydrolyzed silane coupling agent M8:

[0126] The silane coupling agent γ-mercaptopropyltrimethoxysilane and water were mixed in a weight ratio of 3:1. The mixture was then stirred and reacted at 35°C for 2.5 hours until the mixed solution became colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M8.

[0127] Modified silane coupling agent K8 is a combination of hydrolyzed silane coupling agent M8 and silane coupling agent γ-aminopropyltriethoxysilane, wherein the weight ratio of hydrolyzed silane coupling agent M8 to silane coupling agent γ-aminopropyltriethoxysilane is 5:2.

[0128] Preparation of epoxy resin molding compound S8:

[0129] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K8, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 95°C for 9 minutes. The melt-mixed material is cooled, crushed and caked.

[0130] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 40°C for 10 hours.

[0131] Example 9

[0132] The raw materials for preparing epoxy resin molding compound S9 are as follows: the epoxy resin is o-cresol epoxy resin, grade SQCN700-3; the phenolic resin is linear phenolic resin, grade PF5090; the curing accelerators are 2-undecylimidazole and 2-ethyl-4-methylimidazole, wherein the weight ratio of 2-undecylimidazole to 2-ethyl-4-methylimidazole is 9:11; the inorganic filler is silica; the silane coupling agent is γ-aminopropyltriethoxysilane and γ-mercaptopropyltrimethoxysilane; the release agent is carnauba wax; the flame retardant is zinc borate; the modifier is liquid silicone oil; and the colorant is carbon black. The amounts of the raw materials are shown in Table 1.

[0133] Preparation of hydrolyzed silane coupling agent M9:

[0134] The silane coupling agent γ-aminopropyltriethoxysilane and water were mixed in a weight ratio of 3:1. The mixture was then stirred and reacted at 35°C for 2.5 hours until the mixed solution was colorless and transparent, thus obtaining the hydrolyzed silane coupling agent M9.

[0135] Modified silane coupling agent K9 is a combination of hydrolyzed silane coupling agent M9 and silane coupling agent γ-mercaptopropyltrimethoxysilane, wherein the weight ratio of hydrolyzed silane coupling agent M9 to silane coupling agent γ-mercaptopropyltrimethoxysilane is 21:34.

[0136] Preparation of epoxy resin molding compound S9:

[0137] (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent, modified silane coupling agent K9, flame retardant, colorant and modifier are mixed to obtain a mixture. Then the mixture is melt-mixed in an open rubber mixing mill at a temperature of 80°C for 12 minutes. The melt-mixed material is then cooled, crushed and caked.

[0138] (2) The material obtained in step (1) is subjected to a reheating treatment at a temperature of 40°C for 10 hours.

[0139] Comparative Example 1

[0140] The method was implemented according to Example 1, except that an equal weight of silane coupling agent was used instead of modified silane coupling agent K1.

[0141] Comparative Example 2

[0142] The method of Example 1 is implemented, except that step (2) is omitted.

[0143] Comparative Example 3

[0144] The method of Example 1 was implemented, except that an equal weight of silane coupling agent was used to replace the modified silane coupling agent K1, and step (2) was not performed.

[0145] Comparative Example 4

[0146] The method was implemented according to Example 4, except that an equal weight of silane coupling agent was used instead of hydrolyzed silane coupling agent K4.

[0147] Comparative Example 5

[0148] The method of Example 4 is implemented, except that step (2) is omitted.

[0149] Comparative Example 6

[0150] The method of Example 4 was implemented, except that an equal weight of silane coupling agent was used instead of hydrolyzed silane coupling agent K4, and step (2) was not performed.

[0151] Test case

[0152] The samples prepared in the examples and comparative examples were subjected to performance tests. The main test indicators included gelation time, spiral flow length, copper surface adhesion, and surface porosity. The test results are shown in Table 2. All samples were tested using the following methods:

[0153] (1) Gelation time: Hot plate method, heat the electric hot plate to 175±1℃, take 0.3-0.5g sample, grind it, and then place the obtained powder on the electric hot plate. The powder gradually changes from fluid to colloidal state. The time required for this process is the gelation time.

[0154] (1) Spiral flow length: Take a sample and grind it. Then test the obtained powder of 20±5g. Put the obtained powder into the injection molding machine. Under the conditions of injection pressure of 60bar and injection time of 15s, the powder is injected into a special spiral test mold at 175℃. After curing for 120s, it is taken out and the spiral flow length is read.

[0155] (2) Copper surface adhesion: The sample was ground and 20±5g of the obtained powder was tested. The obtained powder was put into an injection molding machine and injected into a special spiral test mold at 175°C under the conditions of injection pressure of 60 bar and injection time of 15s. Shear force was applied along the sample surface at a speed of 20mm / min. The maximum force value before the encapsulant was separated from the sample was tested. The copper surface adhesion test was performed on 5 samples for each example (or comparative example). The average value of the 5 test results was taken as the copper surface adhesion test result of that example (or comparative example).

[0156] (3) Surface porosity: The semiconductor device was packaged using a sample, and the surface porosity of the packaged semiconductor device was counted under a 40x optical microscope. The average of 20 counts was taken as the surface porosity test result of this example (or comparative example).

[0157] Table 2

[0158]

[0159]

[0160] As can be seen from the results in Table 2, the epoxy resin encapsulation material prepared by the method described in this invention has the necessary flowability and adhesion properties. When used to encapsulate semiconductor devices, the encapsulated semiconductor devices have very low surface porosity and better performance. Therefore, epoxy resin encapsulation materials have a promising application prospect in the field of semiconductor packaging.

[0161] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A method for preparing epoxy resin molding compound, characterized in that, The method includes the following steps: (1) Epoxy resin, phenolic resin, curing accelerator, inorganic filler, release agent and modified silane coupling agent, as well as optional flame retardant, optional colorant and optional modifier are mixed and then melt-blended. (2) The material obtained in step (1) is subjected to a reheating treatment; The modified silane coupling agent includes a hydrolyzed silane coupling agent and an optional silane coupling agent; the preparation method of the hydrolyzed silane coupling agent is as follows: the silane coupling agent and water are mixed and then reacted; In step (1), the raw materials for preparing the epoxy resin molding compound contain 6-19% by weight of epoxy resin, 3-9% by weight of phenolic resin, 0.1-0.5% by weight of curing accelerator, 70-87% by weight of inorganic filler, 0.2-1% by weight of release agent, 0.2-0.8% by weight of modified silane coupling agent, 0-8% by weight of flame retardant, 0-1% by weight of colorant and 0-1% by weight of modifier; The curing accelerator is selected from two or more of one of 2-methylimidazole, 2,4-dimethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-butylimidazole, 2-undecylimidazole, 2-phenyl-4-methylimidazole, triphenylphosphine, 1,8-diazabicycloundec-7-ene and triphenylphosphine-1,4-benzoquinone; In step (2), the conditions for the rewarming treatment include: a temperature of 30 to 40°C and a time of 10 to 20 hours.

2. The method according to claim 1, characterized in that, In the method for preparing hydrolyzed silane coupling agents, the weight ratio of silane coupling agent to water is 2 to 5:

1.

3. The method according to claim 1 or 2, characterized in that, The reaction conditions include a temperature of 25–55°C and a time of 0.5–4 h.

4. The method according to claim 1, characterized in that, When the modified silane coupling agent is a hydrolyzed silane coupling agent and a silane coupling agent, the weight ratio of the hydrolyzed silane coupling agent to the silane coupling agent is 0.5-2.5:

1.

5. The method according to claim 1, characterized in that, The silane coupling agent is selected from one or more of γ-glycidoxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-aminopropyltrimethoxysilane, methyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, and N-phenyl-3-aminopropyltrimethoxysilane.

6. The method according to claim 1, characterized in that, The epoxy resin is selected from one or more of the following: o-cresol epoxy resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin, polyphenolic glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, alicyclic epoxy resin, and heterocyclic epoxy resin.

7. The method according to claim 1 or 6, characterized in that, The phenolic resin is selected from one or more of the following: linear phenolic resin and its derivatives, linear phenolic resin and its derivatives, monohydroxy or dihydroxynaphthol phenolic resin and its derivatives, condensates of p-xylene and phenol, condensates of p-xylene and naphthol, and copolymers of dicyclopentadiene and phenol.

8. The method according to claim 1, characterized in that, The inorganic filler is selected from one or more of alumina, titanium dioxide, silicon nitride, aluminum nitride, and silicon dioxide.

9. The method according to claim 1 or 8, characterized in that, The release agent is selected from one or more of carnauba wax, synthetic wax, and paraffin wax.

10. The method according to claim 1, characterized in that, The flame retardant is selected from one or more of the following: halogenated flame retardants, phosphorus-based flame retardants, nitrogen-based flame retardants, phosphorus-halogenated flame retardants, phosphorus-nitrogenated flame retardants, and hydroxide flame retardants.

11. The method according to claim 1, characterized in that, The colorant is selected from one or more of titanium dioxide, zinc oxide, zinc barium white and carbon black.

12. The method according to claim 1, characterized in that, The modifier is liquid silicone oil and / or silicone rubber.

13. An epoxy resin molding compound prepared by the method according to any one of claims 1-12.

14. The application of the epoxy resin encapsulation material according to claim 13 in the field of semiconductor packaging.

Images