WO2024055959A1 - 树脂组合物及其应用 - Google Patents

树脂组合物及其应用 Download PDF

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Publication number
WO2024055959A1
WO2024055959A1 PCT/CN2023/118230 CN2023118230W WO2024055959A1 WO 2024055959 A1 WO2024055959 A1 WO 2024055959A1 CN 2023118230 W CN2023118230 W CN 2023118230W WO 2024055959 A1 WO2024055959 A1 WO 2024055959A1
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Prior art keywords
resin composition
inorganic filler
packaging
epoxy resin
present application
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2023/118230
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English (en)
French (fr)
Inventor
曾志雄
刘成杰
袁灿
金松
包旭升
周慧慧
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huawei Technologies Co Ltd
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Huawei Technologies Co Ltd
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Filing date
Publication date
Application filed by Huawei Technologies Co Ltd filed Critical Huawei Technologies Co Ltd
Priority to EP23864691.3A priority Critical patent/EP4574917A4/en
Publication of WO2024055959A1 publication Critical patent/WO2024055959A1/zh
Priority to US19/080,467 priority patent/US20250206942A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/32—Epoxy compounds containing three or more epoxy groups
    • C08G59/3227—Compounds containing acyclic nitrogen atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5033—Amines aromatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
    • C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
    • C08G65/2627—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aromatic or arylaliphatic amine groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00—Encapsulations, e.g. protective coatings
    • H10W74/40—Encapsulations, e.g. protective coatings characterised by their materials
    • H10W74/47—Encapsulations, e.g. protective coatings characterised by their materials comprising organic materials, e.g. plastics or resins
    • H10W74/473—Encapsulations, e.g. protective coatings characterised by their materials comprising organic materials, e.g. plastics or resins containing a filler
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the embodiments of the present application relate to the technical field of electronic device preparation, and in particular to a resin composition and its application.
  • the packaging gap is getting smaller and smaller (less than 40 ⁇ m), and the packaging interface is becoming more complex. , so the packaging material is required to have narrow gap filling capabilities to achieve narrow gap filling.
  • embodiments of the present application provide a resin composition that has narrow gap filling capabilities and can be used as a packaging material for packaging electronic components, so as to solve the problem of narrow gap filling in existing packaging materials to a certain extent. The problem.
  • the first aspect of the embodiment of the present application provides a resin composition.
  • the resin composition includes an epoxy resin, a curing agent and an inorganic filler.
  • the cut-off particle size of the inorganic filler is 3 ⁇ m, and the D10 of the inorganic filler is 3 ⁇ m. It is 0.1 ⁇ m-0.4 ⁇ m, D50 is 0.5 ⁇ m-1.1 ⁇ m, and D90 is 1.3 ⁇ m-2.9 ⁇ m.
  • the resin composition provided in the embodiment of the present application is liquid at room temperature and is a liquid resin composition. Specifically, it is a liquid epoxy resin composition.
  • the resin composition is made by selecting an inorganic filler with a cut-off particle size of 3 ⁇ m and adding The D10, D50 and D90 of the inorganic filler are controlled within a specific size range, because the inorganic filler has a smaller cut-off particle size, and due to the specific particle size distribution control, the resin composition still has the characteristics of adding a larger amount of small particle size inorganic filler.
  • the low viscosity and high fluidity ultimately enable the resin composition to have good narrow gap packaging filling capabilities.
  • the resin composition is used as an underfill material to be filled between electronic components (such as chips), solder bumps and substrates to form an underfill adhesive layer, which can meet the filling requirements of narrow packaging gaps less than 40 ⁇ m and can also better avoid bottom filling.
  • the pores are generated during filling to prevent the inorganic filler from settling, so that the formed bottom filling glue layer has a higher uniformity, thereby improving the packaging reliability, improving the service reliability of electronic components, and better matching the increasingly narrower and narrower electronic packaging field.
  • the underfill glue layer can disperse the stress carried on the surface of electronic components, alleviate the internal stress problem caused by the mismatch of thermal expansion coefficient CTE between the chip, the soldering bumps and the substrate, protect the soldering bumps, and ensure the reliable operation of electronic components.
  • the D10 of the inorganic filler is 0.2 ⁇ m-0.3 ⁇ m
  • the D50 is 0.6 ⁇ m-1.0 ⁇ m
  • the D90 is 1.5 ⁇ m-2.7 ⁇ m.
  • Controlling the D10, D50 and D90 of the inorganic filler within the above-mentioned specific size range is beneficial for the resin composition to still have low viscosity and high fluidity even when a larger amount of small particle size inorganic filler is added, and improves the narrow gap encapsulation of the resin composition.
  • the filling capacity can also better avoid the formation of pores during underfilling, prevent the inorganic filler from settling, and make the formed underfill layer more uniform, thereby improving packaging reliability and improving the service reliability of electronic components.
  • Appropriate particle size distribution coefficient control is conducive to better improving the narrow gap encapsulation filling ability of the resin composition system.
  • the specific surface area of the inorganic filler is 2m 2 /g-10m 2 /g. Controlling the specific surface area of the inorganic filler within a suitable range can enhance the interaction between the inorganic filler and the epoxy resin, better prevent the inorganic filler from settling, and prevent the inorganic filler from settling when the resin composition is used for underfilling.
  • the filler and epoxy resin are more evenly distributed, thus making the performance of the underfill glue layer more uniform, which ultimately helps improve packaging reliability and improve the service reliability of electronic components.
  • the inorganic filler includes one or more of silicon dioxide, aluminum oxide, magnesium oxide, aluminum nitride, and silicon nitride.
  • the addition of these inorganic fillers can reduce the thermal expansion coefficient of the resin composition system and reduce thermal stress, and can also reduce water absorption, reduce molding shrinkage, reduce resin overflow, improve mechanical properties, increase thermal deformation temperature, and enhance wear resistance.
  • the inorganic filler is a spherical particle with a sphericity greater than 98%.
  • the mass proportion of the inorganic filler is greater than or equal to 55%.
  • the mass proportion of the inorganic filler in the resin composition is 55%-80%.
  • the resin composition can better balance low thermal expansion coefficient, high glass transition temperature Tg, low viscosity and suitable mechanical properties, thereby ensuring that the resin composition can be used as an underfill material. Narrow gap underfill improves packaging reliability.
  • the epoxy resin includes glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, aliphatic epoxy resin, bisphenol F epoxy resin, One or more of naphthalene-type epoxy resin, aminophenol-type epoxy resin, binaphthyl-type epoxy resin, bisphenol-A-type epoxy resin, and phenolic-type epoxy resin.
  • the epoxy resin may be one type or a combination of multiple types (two or more types).
  • the epoxy resin includes a multifunctional epoxy resin. Multifunctional (trifunctional or above) epoxy resin is cross-linked with the curing agent, which can increase the overall cross-linking density of the cured product and increase the glass transition temperature Tg of the cured product of the resin composition, thereby improving packaging reliability and effectively avoiding The occurrence of chip failure problems improves the reliability of high junction temperature chips.
  • the mass proportion of the curing agent in the resin composition is 5%-20%.
  • Appropriate curing agent content can enable the epoxy resin to be cured smoothly and obtain the basic physical properties that meet the packaging requirements.
  • the mass proportion of the epoxy resin in the resin composition is 15%-30%.
  • a suitable epoxy resin content can enable the resin composition to meet the basic physical properties of the package, achieve filling, and better ensure a strong bond between the chip, solder bumps and substrate.
  • the curing agent includes an amine curing agent and/or an acid anhydride curing agent.
  • the acid anhydride curing agent may be hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, alkyl hexahydrophthalic anhydride, tetrahydrophthalic anhydride, One of hydrogen phthalic anhydride, succinic anhydride, methyl nadic anhydride, hydrogenated methyl nadic anhydride, 5-norbornene-2,3-dioic anhydride, trialkyl tetrahydrophthalic anhydride, etc.
  • the amine curing agent can be an aromatic amine curing agent or an aliphatic amine curing agent.
  • the amine curing agent can be diethyltoluenediamine, polyetheramine, isophor Ketone diamine, 3,3'-dimethyl-4,4'-diamino-dicyclohexylmethane, etc.
  • the resin composition in order to improve the performance of the resin composition, may also include additives.
  • the additives include coupling agents, toughening agents, stress modifiers, curing accelerators, colorants, and dispersants. , one or more of ion trapping agents, defoaming agents, leveling agents, flame retardants, release agents, and flow improvers. Additives can be added according to specific needs.
  • the viscosity of the resin composition at 110°C is less than 0.3 Pa.s.
  • the resin composition has a lower viscosity, which is conducive to ensuring that the resin composition has good fluidity and filling properties during packaging and filling, thereby better meeting the narrow gap filling requirements and improving the packaging effect.
  • the glass transition temperature of the cured product of the resin composition is greater than or equal to 145°C.
  • the resin composition has a high glass transition temperature Tg after curing, which can improve the service reliability of the adhesive layer obtained by encapsulation and effectively avoid chip failure problems.
  • the thermal expansion coefficient of the cured product of the resin composition is 25 ppm/°C-35 ppm/°C. A lower thermal expansion coefficient helps improve packaging reliability.
  • the second aspect of the embodiment of the present application provides a packaging material for sealed packaging (ie, packaging) of electronic components.
  • the packaging material includes the resin composition and/or the resin described in the first aspect of the embodiment of the present application.
  • the cured product of the composition Using the resin composition provided in the embodiments of the present application as a packaging material (ie, electronic packaging material) for packaging electronic components can improve the packaging effect and improve the service reliability of electronic devices.
  • the third aspect of the embodiments of the present application provides the application of the resin composition described in the first aspect in sealed packaging of electronic components. That is, the application of the resin composition as an electronic packaging material in the field of electronic packaging.
  • the application of the resin composition in sealed packaging of electronic components may include the resin composition as the bottom Application of filling materials in sealed packaging of electronic components.
  • the resin composition is filled between the substrate and the electronic components, and a strong filling layer is formed after heating and solidification, which can reduce the stress impact caused by the difference in thermal expansion coefficient between the electronic components and the substrate and improve the strength of the packaging structure. and connection reliability, enhancing the overall anti-drop performance of the packaging structure.
  • the fourth aspect of the embodiments of the present application provides a cured product, which includes a cured product of the resin composition described in the first aspect of the embodiments of the present application.
  • the cured product in the embodiment of the present application may be filled between the substrate and the electronic component, specifically between the solder bumps connecting the substrate and the electronic component.
  • the fifth aspect of the embodiment of the present application provides a packaged device, which includes the cured product described in the fourth aspect of the embodiment of the present application.
  • the device encapsulated in the embodiments of this application is encapsulated using the cured product of the resin composition provided in the embodiments of this application, and has high service reliability.
  • the package device includes a substrate and an electronic component arranged on the substrate.
  • a plurality of welding bumps are provided on a side surface of the electronic component facing the substrate.
  • the welding bumps There is an underfill glue layer between them, and the underfill glue layer includes the cured product.
  • the package device further includes a plastic encapsulation body covering the surface of the electronic component.
  • electronic components include but are not limited to chips. When the electronic components are chips, the packaging device is a chip packaging structure.
  • An embodiment of the present application also provides a terminal device, which includes a circuit board and the packaging device described in the fifth aspect of the embodiment of the present application provided on the circuit board.
  • the terminal equipment of the embodiment of the present application can improve the service reliability of the terminal equipment by using the packaging device provided by the embodiment of the present application.
  • An embodiment of the present application further provides a communication device, which includes the packaging device described in the fifth aspect of the embodiment of the present application.
  • An embodiment of the present application also provides a communication base station, which includes the packaging device described in the fifth aspect of the embodiment of the present application.
  • Figure 1 is a schematic structural diagram of a package device 100 provided by an embodiment of the present application.
  • Figure 2 is a schematic diagram of the packaged device 100 arranged on a circuit board according to the embodiment of the present application;
  • FIG. 3 is a schematic structural diagram of a terminal device 200 provided by an embodiment of the present application.
  • Packaging material between the substrate and the chip and forming a strong bottom filling adhesive layer after heat curing can reduce the stress impact caused by the difference in thermal expansion coefficient between the chip and the substrate, protect the chip, substrate and welding bumps, and improve the packaging structure.
  • the strength and connection reliability improve the overall drop resistance of the packaging structure.
  • the packaging gap is getting smaller and smaller (less than 40 ⁇ m), and the packaging interface is becoming more complex. Therefore, packaging materials are required to have excellent narrow gap filling capabilities and better match.
  • the electronic packaging field is getting narrower and more complex with narrow gap packaging application requirements.
  • embodiments of the present application provide a resin composition, which is in a liquid state and is a liquid encapsulation material.
  • the resin composition has good narrow gap encapsulation filling ability.
  • the resin composition can be used in, but is not limited to, flip chip, fan-in wafer-level packaging FOWLP, fan-out wafer-level packaging FOWLP, through silicon via technology TSV, 2.5D packaging, 3D packaging, embedded In advanced packaging structures such as wafer-level ball grid array packaging eWLB.
  • the embodiment of the present application provides a resin composition, which includes an epoxy resin, a curing agent and an inorganic filler, wherein the cut-off particle size of the inorganic filler is 3 ⁇ m, the D10 of the inorganic filler is 0.1 ⁇ m-0.4 ⁇ m, and the D50 is 0.5 ⁇ m-1.1 ⁇ m, D90 is 1.3 ⁇ m-2.9 ⁇ m.
  • the cut-off particle size that is, the cut-off particle size and the cut-off particle size
  • the cut-off particle size and the cut-off particle size is the theoretical maximum particle size.
  • the cut-off particle size of inorganic fillers is 3 ⁇ m, which means that the particle size is basically less than or equal to 3 ⁇ m, and the particle size is greater than 3 ⁇ m and is in the ppm level.
  • the resin composition provided in the embodiment of the present application is liquid at room temperature and is a liquid resin composition. Specifically, it is a liquid epoxy resin composition.
  • the resin composition is made by selecting an inorganic filler with a cut-off particle size of 3 ⁇ m and adding The D10, D50 and D90 of the inorganic filler are controlled within a specific size range, because the inorganic filler has a smaller cut-off particle size, and due to the specific particle size distribution control, the resin composition still has the characteristics of adding a larger amount of small particle size inorganic filler.
  • the low viscosity and high fluidity ultimately enable the resin composition to have good narrow gap packaging filling capabilities.
  • the resin composition is used as an underfill material to be filled between electronic components (such as chips), solder bumps and substrates to form an underfill adhesive layer, which can meet the filling requirements of narrow packaging gaps less than 40 ⁇ m and can also better avoid bottom filling.
  • the pores are generated during filling to prevent the inorganic filler from settling, so that the formed bottom filling glue layer has a higher uniformity, thereby improving the packaging reliability, improving the service reliability of electronic components, and better matching the increasingly narrower and narrower electronic packaging field.
  • the underfill glue layer can disperse the stress carried on the surface of electronic components, alleviate the internal stress problem caused by the mismatch of thermal expansion coefficient CTE between the chip, the soldering bumps and the substrate, protect the soldering bumps, and ensure the reliable operation of electronic components.
  • the D10 of the inorganic filler is 0.1 ⁇ m-0.4 ⁇ m
  • the D50 is 0.5 ⁇ m-1.1 ⁇ m
  • the D90 is 1.2 ⁇ m-2.9 ⁇ m.
  • D10 may be, for example, 0.1 ⁇ m, 0.2 ⁇ m, 0.3 ⁇ m, or 0.4 ⁇ m
  • D50 may be, for example, 0.5 ⁇ m, 0.6 ⁇ m, 0.7 ⁇ m, 0.8 ⁇ m, 0.9 ⁇ m, 1.0 ⁇ m, or 1.1 ⁇ m
  • D90 may be, for example, 1.3 ⁇ m.
  • the inorganic filler has a D10 of 0.2 ⁇ m-0.3 ⁇ m, a D50 of 0.6 ⁇ m-1.0 ⁇ m, and a D90 of 1.5 ⁇ m-2.7 ⁇ m.
  • D10, D50 and D90 are the particle sizes corresponding to when the cumulative particle size distribution numbers reach 10%, 50% and 90% respectively.
  • Controlling the D10, D50 and D90 of the inorganic filler within the above-mentioned specific size range is beneficial for the resin composition to still have low viscosity and high fluidity even when a larger amount of small particle size inorganic filler is added, and improves the narrow gap encapsulation of the resin composition.
  • the filling capacity can also better avoid the formation of pores during underfilling, prevent the inorganic filler from settling, and make the formed underfill layer more uniform, thereby improving packaging reliability and improving the service reliability of electronic components.
  • the particle size value of the inorganic filler in the embodiments of the present application may have errors allowed by detection methods or detection instruments in this field.
  • the particle size distribution coefficient P of the inorganic filler is 1-3.5.
  • the particle size distribution coefficient P of the inorganic filler may be, for example, 1, 1.5, 2, 2.3, 2.5, 2.7, 3, or 3.5. Appropriate particle size distribution coefficient control is conducive to better improving the narrow gap encapsulation filling ability of the resin composition system.
  • the specific surface area of the inorganic filler is 2m 2 /g-10m 2 /g.
  • Specific surface area refers to the total area per unit mass of material.
  • the specific surface area of the inorganic filler can specifically be 2m 2 /g, 3m 2 /g, 4m 2 / g, 5m 2 /g, 6m 2 /g, 7m 2 /g, 8m 2 /g, 9m 2 /g, 10m 2 /g.
  • Controlling the specific surface area of the inorganic filler within a suitable range can enhance the interaction between the inorganic filler and the epoxy resin, better prevent the inorganic filler from settling, and prevent the inorganic filler from settling when the resin composition is used for underfilling.
  • the filler and epoxy resin are more evenly distributed, thus making the performance of the underfill glue layer more uniform, which ultimately helps improve packaging reliability and improve the service reliability of electronic components.
  • the inorganic filler may include one or more of silica, alumina, magnesium oxide, aluminum nitride, and silicon nitride.
  • the addition of these inorganic fillers can reduce the thermal expansion coefficient of the resin composition system and reduce thermal stress. It can also reduce water absorption, reduce molding shrinkage, reduce resin flash, improve mechanical properties, increase thermal deformation temperature and enhance wear resistance, thereby improving Encapsulation reliability of resin composition used as encapsulation material.
  • the inorganic filler is a spherical particle with a sphericity greater than 98%.
  • the inorganic filler is spherical silica.
  • the use of spherical silica is beneficial to better improving the fluidity and thermal expansion coefficient of the resin composition.
  • the cut-off particle size of the inorganic filler can be measured by scanning electron microscope (SEM), etc.; the particle size distribution of the inorganic filler can be analyzed by a dynamic light scattering particle size analyzer.
  • the mass proportion of the inorganic filler in the resin composition is greater than or equal to 55%.
  • the mass proportion of the inorganic filler in the resin composition is 55%-80%. In some embodiments of the present application, the mass proportion of inorganic fillers in the resin composition is 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65 %, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 75%, 80%.
  • the resin composition can better balance low thermal expansion coefficient, high glass transition temperature Tg, low viscosity and suitable mechanical properties, thereby ensuring that the resin composition can be used as an underfill material. Narrow gap underfill improves packaging reliability.
  • the epoxy resin may include glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, aliphatic epoxy resin, bisphenol F epoxy resin, One or more of naphthalene-type epoxy resin, aminophenol-type epoxy resin, binaphthyl-type epoxy resin, bisphenol-A-type epoxy resin, and phenolic-type epoxy resin.
  • the epoxy resin may be one type or a combination of multiple types (two or more types).
  • the epoxy resin includes one of bisphenol F epoxy resin, aminophenol epoxy resin, bisphenol A epoxy resin, naphthalene epoxy resin, binaphthyl epoxy resin, or Various.
  • the type of epoxy resin and the type of curing agent can be obtained through analysis using nuclear magnetic resonance spectroscopy, infrared spectroscopy, elemental analysis and other methods.
  • the epoxy resin includes a multifunctional epoxy resin. Multifunctional (trifunctional and above) epoxy resin is cross-linked with the curing agent, which can increase the overall cross-linking density of the cured product and improve the resin composition.
  • the glass transition temperature Tg of the solidified product is thereby improved, thereby improving packaging reliability, effectively avoiding chip failure problems, and improving the reliability of high junction temperature chips.
  • the mass proportion of the curing agent in the resin composition is 5%-20%. In some embodiments of the present application, the mass proportion of the curing agent in the resin composition may be 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%. Appropriate curing agent content can enable the epoxy resin to be cured smoothly and obtain the basic physical properties that meet the packaging requirements.
  • the mass proportion of epoxy resin in the resin composition is 15%-30%. In some embodiments of the present application, the mass proportion of epoxy resin in the resin composition can be 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24% , 25%, 26%, 27%, 28%, 29%, 30%.
  • a suitable epoxy resin content can enable the resin composition to meet the basic physical properties of the package, achieve filling, and better ensure a strong bond between the chip, solder bumps and substrate.
  • the curing agent may include an amine curing agent and/or an acid anhydride curing agent.
  • the acid anhydride curing agent may be hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, alkyl hexahydrophthalic anhydride, tetrahydrophthalic anhydride, One of hydrogen phthalic anhydride, succinic anhydride, methyl nadic anhydride, hydrogenated methyl nadic anhydride, 5-norbornene-2,3-dioic anhydride, trialkyl tetrahydrophthalic anhydride, etc.
  • the amine curing agent can be an aromatic amine curing agent or an aliphatic amine curing agent.
  • the amine curing agent can be diethyltoluenediamine, polyetheramine, isophor One or more of ketone diamine, 3,3'-dimethyl-4,4'-diamino-dicyclohexylmethane, etc.
  • amine curing agents have lower water absorption, which is beneficial to reducing the water absorption rate of the cured product of the resin composition.
  • the resin composition of the present application may include one curing agent or multiple (two or more) curing agents.
  • the resin composition in order to improve the performance of the resin composition, may also include additives.
  • the additives include but are not limited to coupling agents, toughening agents, stress modifiers, curing accelerators, colorants, One or more of dispersants, ion trapping agents, defoaming agents, leveling agents, flame retardants, release agents, and flow improvers. Additives can be added according to specific needs.
  • coupling agents, toughening agents, stress modifiers, curing accelerators, colorants, dispersants, ion trapping agents, defoaming agents, leveling agents, flame retardants, release agents, flow The specific type of improver is not particularly limited.
  • coupling agents include but are not limited to ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ -methacryloyloxypropyltrimethoxysilane, 3- One or more of aminopropyltrimethoxysilane and N-( ⁇ -aminoethyl)- ⁇ -aminopropyltrimethoxysilane.
  • Curing accelerators include but are not limited to one of tertiary amines (such as N,N-dimethylbenzeneamine, etc.), imidazole, modified imidazole (such as dimethylimidazole, 1-phenyldimethylimidazole, etc.) or Various.
  • the viscosity of the resin composition at 110°C is less than 0.3 Pa.s.
  • the viscosity of the resin composition can be tested using a rheometer.
  • the viscosity of the resin composition at 110°C is less than 0.25 Pa.s.
  • the viscosity of the resin composition at 110°C is less than 0.2 Pa.s.
  • the viscosity of the resin composition at 110°C is less than 0.15 Pa.s.
  • the viscosity of the resin composition can be tested using a rheometer. It should be noted that the resin compositions in the examples of the present application need to be stored and transported at low temperatures of -40°C and below.
  • the above viscosity refers to the viscosity measured just after the resin composition is prepared, or the viscosity measured after thawing.
  • the resin composition has a lower viscosity, which is conducive to ensuring that the resin composition has good fluidity and filling properties during packaging and filling, thereby better meeting the narrow gap filling requirements and improving the packaging effect.
  • the glass transition temperature of the cured product of the resin composition is greater than or equal to 145°C. In some embodiments of the present application, the glass transition temperature of the cured product of the resin composition is greater than or equal to 150°C. In some embodiments of the present application, the glass transition temperature of the cured product of the resin composition is greater than or equal to 160°C. In some embodiments of the present application, the glass transition temperature of the cured product of the resin composition is greater than or equal to 170°C. In some embodiments of the present application, the glass transition temperature of the cured product of the resin composition is greater than or equal to 180°C.
  • the resin composition has a high glass transition temperature Tg after curing, which can improve the service reliability of the adhesive layer obtained by encapsulation and effectively avoid chip failure problems.
  • the thermal expansion coefficient of the cured product of the resin composition is 25 ppm/°C-35 ppm/°C.
  • the thermal expansion coefficient of the cured product of the resin composition may be, for example, 25 ppm/°C, 26 ppm/°C, 27 ppm/°C, 28 ppm/°C, 29 ppm/°C, 30 ppm/°C, 31 ppm/°C, 32 ppm/°C, or 33 ppm/°C. , 34ppm/°C, 35ppm/°C.
  • a lower thermal expansion coefficient helps improve packaging reliability.
  • the resin composition in the embodiment of the present application can be prepared by stirring and mixing each component. Stirring and mixing can be performed solely with an overhead mechanical mixer, dual planetary mixer, homogenizer, or three-roller grinder, or a combination of the above devices can be used.
  • the resin composition in the embodiment of the present application is a liquid packaging material, which can be filled into a syringe of 10cc, 30cc or larger volume for storage.
  • the resin composition of the embodiment of the present application needs to be stored and transported at a low temperature of -40°C and below.
  • the resin composition in the embodiment of the present application will be cured when heated, and the epoxy resin and the curing agent in the resin composition can react chemically to form a three-dimensional network polymer.
  • the resin composition is converted into a cured product of a certain shape after curing, and the cured product may be in the form of a film, a sheet, or a three-dimensional structure.
  • the resin composition mentioned above in this application is usually in liquid state.
  • the liquid resin composition can be directly used as liquid glue, and can be coated, filled, and cured to form a glue layer.
  • the resin composition in the embodiment of the present application is an epoxy resin composition containing inorganic fillers, and the resin composition has good narrow gap encapsulation and filling capabilities.
  • the resin composition can be used as an underfill material to be filled between electronic components (such as chips), solder bumps and substrates to form an underfill adhesive layer, which can meet the filling requirements of narrow packaging gaps of 40 ⁇ m and below, and can also better avoid Air holes are generated during underfilling, which prevents the inorganic filler from settling and makes the formed underfill glue layer highly uniform, thereby improving packaging reliability and improving the service reliability of electronic components.
  • the resin composition can be used in, but is not limited to, flip chip, fan-in wafer-level packaging FOWLP, fan-out wafer-level packaging FOWLP, through silicon via technology TSV, 2.5D packaging, and 3D packaging.
  • embedded wafer-level ball grid array packaging, eWLB and other advanced packaging structures products using these advanced packaging structures (such as processors, etc.) can be used in mobile phones, computers, automobiles and other complete equipment.
  • the resin composition of the present application can also be used in large-area molding, thin grinding-free packaging, passive devices and POP (package-on-package, package stacking technology) packaging, etc. These packaging products can be used in wireless wireless devices for mobile electronic devices. devices and self-driven sensors.
  • Embodiments of the present application also provide a packaging material.
  • the packaging material is an electronic packaging material and is used for sealed packaging of electronic components.
  • the packaging material includes the resin composition provided above in the embodiment of the present application and/or the resin combination provided above. solidified substance. Using the resin composition provided above in the embodiments of the present application as a packaging material for packaging electronic components can improve the packaging effect and improve the service reliability of electronic components.
  • the embodiments of the present application provide the application of the above-mentioned resin composition in the field of electronic packaging, that is, the application of the resin composition as an electronic packaging material in the field of electronic packaging.
  • electronic components may be chips, transistors (such as diodes, transistors), LEDs, resistor-capacitor components (such as resistors, capacitors, inductors), etc.
  • the structural form of packaging can be flip chip, fan-in wafer level packaging FOWLP, fan-out wafer level packaging FOWLP, through silicon via technology TSV, 2.5D packaging, 3D packaging, embedded wafer level Advanced packaging structures such as ball grid array packaging eWLB can also be packaged in large-area molding, thin no-grinding packaging, passive device packaging, and POP (package-on-package, package stacking technology) packaging.
  • the application of the resin composition in the sealed packaging of electronic components may include the application of the resin composition as an underfill material in the sealed packaging of electronic components.
  • the resin composition is filled between the substrate and the electronic components, and a strong filling layer is formed after heating and solidification, which can reduce the stress impact caused by the difference in thermal expansion coefficient between the electronic components and the substrate and improve the strength of the packaging structure. and connection reliability, enhancing the overall anti-drop performance of the packaging structure.
  • the embodiments of the present application also provide a cured product, which includes the cured product of the resin composition described above in the embodiments of the present application.
  • the cured product in the embodiment of the present application may be filled between the substrate and the electronic component, specifically between the solder bumps connecting the substrate and the electronic component.
  • the cured product can be in the shape of film, sheet, three-dimensional structure, etc.
  • the cured product has the characteristics of low thermal expansion coefficient CTE, high glass transition temperature Tg, high mechanical strength, low water absorption and other characteristics.
  • FIG. 1 is a schematic structural diagram of the packaging device 100 in an embodiment of the present application.
  • the packaged device 100 may be an electronic device package, and the packaged device 100 includes the cured product of the resin composition described in the embodiment of the present application.
  • the packaged device 100 includes a substrate 10 and an electronic component 20 disposed on the substrate 10.
  • the electronic component 20 is provided with a plurality of soldering bumps 30 on one side of the surface facing the substrate 10.
  • the substrate 10 is located between the soldering bumps 30.
  • An underfill glue layer 40 is provided between the electronic component 20 and the welding bump 30.
  • the underfill glue layer 40 includes the cured product of the resin composition described in the embodiment of the present application.
  • the packaged device 100 further includes a plastic encapsulation body 60 covering the surface of the electronic component 200 .
  • the soldering bumps 30 are electrically connected to the electronic components 20 through the conductive structures 50 in the substrate 10 .
  • the electronic component 20 can be a variety of components that need to be packaged, including but not limited to one of chips, transistors (such as diodes, triodes), LEDs, resistance-capacitance components (such as resistors, capacitors, inductors), etc. or more.
  • the packaging device 100 is a chip packaging structure.
  • the electronic component 20 may be attached to the surface of the substrate 10 through soldering, and the substrate 10 may be a redistribution layer (RDL).
  • RDL redistribution layer
  • the packaged device 100 can be welded to the circuit board 101.
  • a plurality of metal balls 70 can be provided on the side of the substrate 10 away from the electronic components 20.
  • the electronic components 20 in the packaged device 100 can pass through the conductive structure 50, metal
  • the ball 70 is electrically connected to the circuit board 101, and a filling glue layer 80 is provided between the substrate 10, the circuit board 101, and the metal ball 70.
  • the filling glue layer 80 may also be a cured product including the resin composition described in the embodiment of the present application.
  • the packaged device 100 in the embodiment of the present application uses the resin composition provided in the embodiment of the present application to package electronic components, which can achieve narrow gap filling, high process operability, and high packaging reliability.
  • the embodiment of the present application also provides a terminal device 200.
  • the terminal device 200 includes a housing 201, a circuit board and a packaging device 100 disposed in the housing 201. Inside the terminal device 200, the packaging device 100 can be as follows: As shown in FIG. 2 , it is arranged on the circuit board 101 and is electrically connected to the circuit board 101 .
  • the terminal device 200 may be a mobile phone, a tablet computer, a notebook computer, a portable computer, a smart wearable product, a television, a video recorder, a camcorder, a radio, a cassette player, a vehicle-mounted terminal, a mouse, a keyboard, a microphone, a scanner, and other products.
  • An embodiment of the present application also provides a communication device.
  • the communication device includes the packaging device 100 mentioned above in the embodiment of the present application.
  • the packaged device 100 may be electrically connected and fixed on the circuit board.
  • Communication equipment can be various types of wired communication equipment or wireless communication equipment, including but not limited to communication conversion equipment, lightning arresters, antennas, gateways, remote controls, radars, walkie-talkies, switches, routers, etc.
  • An embodiment of the present application also provides a communication base station.
  • the communication base station includes the packaging device 100 described above in the embodiment of the present application.
  • the packaged device 100 may be electrically connected and fixed on the circuit board.
  • a resin composition including the following components by mass: 26% trifunctional aminophenol epoxy resin, 13% aromatic amine curing agent diethyl toluenediamine, 60% inorganic filler A1, coupling agent ⁇ - Glycidyloxypropyltrimethoxysilane 1%, in which the inorganic filler is a spherical silane with a cutoff particle size of 3 ⁇ m, D10 of 0.3 ⁇ m, D50 of 1.0 ⁇ m, D90 of 2.7 ⁇ m, and a specific surface area of 7 m 2 /g. Silicon oxide.
  • a resin composition including the following components by mass: 26% trifunctional aminophenol epoxy resin, 13% aromatic amine curing agent diethyl toluenediamine, 60% inorganic filler A2, coupling agent ⁇ - Glycidyloxypropyltrimethoxysilane 1%, in which the inorganic filler is a spherical shape with a cut-off particle diameter of 3 ⁇ m, D10 of 0.2 ⁇ m, D50 of 0.8 ⁇ m, D90 of 2.4 ⁇ m, and a specific surface area of 7.6 m 2 /g Silica.
  • a resin composition including the following components by mass: 26% trifunctional aminophenol epoxy resin, 13% aromatic amine curing agent diethyl toluenediamine, 60% inorganic filler A3, coupling agent ⁇ - Glycidyloxypropyltrimethoxysilane 1%, in which the inorganic filler is a spherical silane with a cut-off particle size of 3 ⁇ m, D10 of 0.2 ⁇ m, D50 of 0.6 ⁇ m, D90 of 2.0 ⁇ m, and a specific surface area of 8 m 2 /g. Silicon oxide.
  • a resin composition including the following components by mass: 24.5% trifunctional aminophenol epoxy resin, 9.5% aromatic amine curing agent diethyl toluenediamine, 65% inorganic filler A1, coupling agent ⁇ - Glycidyloxypropyltrimethoxysilane 1%, in which the inorganic filler is a spherical silane with a cutoff particle size of 3 ⁇ m, D10 of 0.3 ⁇ m, D50 of 1.0 ⁇ m, D90 of 2.7 ⁇ m, and a specific surface area of 7 m 2 /g. Silicon oxide.
  • a resin composition including the following components by mass: 22.5% trifunctional aminophenol epoxy resin, 6.5% aromatic amine curing agent diethyl toluenediamine, 70% inorganic filler A1, coupling agent ⁇ - Glycidyloxypropyltrimethoxysilane 1%, in which the inorganic filler is a spherical silane with a cutoff particle size of 3 ⁇ m, D10 of 0.3 ⁇ m, D50 of 1.0 ⁇ m, D90 of 2.7 ⁇ m, and a specific surface area of 7 m 2 /g. Silicon oxide.
  • a resin composition including the following components by mass: 15% bisphenol F epoxy resin, 10% trifunctional aminophenol epoxy resin, 9% aromatic amine curing agent diethyl toluenediamine, inorganic Filler A1 65%, coupling agent ⁇ -glycidyl etheroxypropyl trimethoxysilane 1%, in which the inorganic filler has a cut-off particle size of 3 ⁇ m, D10 is 0.3 ⁇ m, D50 is 1.0 ⁇ m, and D90 is 2.7 ⁇ m.
  • the inorganic filler B1 is a spherical particle with a cut-off particle diameter of 5 ⁇ m, D10 of 0.1 ⁇ m, D50 of 1.5 ⁇ m, D90 of 4.8 ⁇ m, and a specific surface area of 6 m 2 /g. Silicon oxide.
  • the inorganic filler B2 is a spherical filler with a cutoff particle size of 3 ⁇ m, D10 of 0.1 ⁇ m, D50 of 0.3 ⁇ m, D90 of 0.9 ⁇ m, and a specific surface area of 9 m 2 /g. Silicon oxide.
  • the viscosity of the resin composition is measured with a rheometer, at 110°C, the viscosity at 50 rpm is taken; the flow length test of the resin composition is measured at a gap of 40 ⁇ m, the flow length at 110°C for 10 minutes; the glass of the cured resin composition
  • the chemical transition temperature Tg is measured using a dynamic thermomechanical analyzer.
  • Examples 1 to 6 of the present application adopted a cutoff particle size of 3 ⁇ m, and D10, D50, and D90 were within specific sizes.
  • the prepared resin composition can obtain low viscosity and a narrow gap flow length greater than or equal to 40 mm, indicating that the resin composition of the embodiment of the present application has high fluidity and good narrow gap filling ability.
  • Comparative Example 1 uses silica with a cut-off particle size of 5 ⁇ m as a filler. The resin composition has a higher viscosity and a shorter flow length in the narrow gap, which is 38 mm.
  • Comparative Example 2 uses a cutoff particle size of 3 ⁇ m, its D10 is 0.1 ⁇ m, D50 is 0.3 ⁇ m, and D90 is 0.9 ⁇ m.
  • the viscosity of the resin composition is high, and the flow length in the narrow gap is short, 30 mm.
  • the resin compositions of Examples 1 to 6 of the present application, as well as Comparative Examples 1 and 2 were used for underfilling of 25mm*25mm sized chips. Ultrasonic scanning was used to characterize the filling glue layer, and the bottom filling glue layer was observed with a scanning electron microscope after slicing. The results showed that the resin compositions of Examples 1 to 6 of the present application can completely fill gaps of 40 ⁇ m and below, with high filling efficiency. And there are no bubbles in the bottom filling glue layer and no filler settlement.
  • the filling efficiency of the resin composition of Comparative Example 1 is low, and it takes longer to achieve complete filling than the resin compositions of Examples 1 to 6, and the bottom filling glue layer has sedimentation of the inorganic filler. However, the resin composition of Comparative Example 2 could not achieve complete filling at all.
  • At least one refers to one or more
  • plural refers to two or more.
  • At least one of the following” or similar expressions thereof refers to any combination of these items, including any combination of a single item (items) or a plurality of items (items).
  • at least one of a, b, or c or “at least one of a, b, and c” can mean: a, b, c, a-b ( That is, a and b), a-c, b-c, or a-b-c, where a, b, and c can be single or multiple respectively.

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Abstract

本申请实施例提供一种树脂组合物，所述树脂组合物包括环氧树脂、固化剂和无机填料，所述无机填料的截止粒径为3μm，所述无机填料的D10为0.1μm-0.4μm，D50为0.5μm-1.1μm，D90为1.3μm-2.9μm。该树脂组合物具有低粘度和高流动性，具备良好的窄间隙填充能力。本申请实施例还提供了该树脂组合物的应用。

Description

树脂组合物及其应用
本申请要求于2022年9月15日提交中国专利局、申请号为202211119850.4、申请名称为“树脂组合物及其应用”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本申请实施例涉及电子器件制备技术领域，特别是涉及一种树脂组合物及其应用。
背景技术
随着信息技术的不断发展，电子整机设备向小型化、便携式、多功能化、数字化及高可靠性、高性能等方向发展，因此要求设备内部元器件趋于小型化、集成化以至模块化。基于此，出现了倒装芯片(Flip chip)、扇入型晶圆级封装(Fan-in Wafer Level Packaging,FOWLP)、扇出型晶圆级封装(Fan-Out Wafer Level Packaging,FOWLP)、硅通孔技术(Through Silicon Via，TSV)、2.5D封装、3D封装、eWLB(Embedded Wafer Level Ball Grid Array，嵌入型晶圆级球栅阵列封装)等先进封装形式。封装材料(如环氧模塑料、芯片粘接胶、底部填充材料、导热胶等)用于在这些封装形式中起绝缘、粘接、缓解应力、保护等作用，确保芯片的可靠性运行。
其中，在2.5D、3D先进封装中，为增加I/O(Input/Ouput接口，即输入/输出接口)数、缩短信号传输距离，封装间隙越来越小(小于40μm)，封装界面愈加复杂，因此要求封装材料具备窄间隙填充能力，以实现窄间隙填充。
发明内容
鉴于此，本申请实施例提供一种树脂组合物，该树脂组合物具备窄间隙填充能力，能够作为封装材料用于电子元器件的封装，以在一定程度上解决现有封装材料窄间隙填充困难的问题。
具体地，本申请实施例第一方面提供一种树脂组合物，所述树脂组合物包括环氧树脂、固化剂和无机填料，所述无机填料的截止粒径为3μm，所述无机填料的D10为0.1μm-0.4μm，D50为0.5μm-1.1μm，D90为1.3μm-2.9μm。
本申请实施例提供的树脂组合物在室温下为液态，为液态树脂组合物，具体是一种液态的环氧树脂组合物，该树脂组合物通过选用截止粒径为3μm的无机填料，并将无机填料的D10、D50和D90控制在特定尺寸范围，由于无机填料具有较小的截止粒径，且由于特定粒径分布控制使得树脂组合物在添加较大量小粒径无机填料的情况下仍具有低粘度和高流动性，最终可使得树脂组合物具有良好的窄间隙封装填充能力。将该树脂组合物作为底部填充材料填充于电子元器件(如芯片)、焊接凸点和基板之间形成底部填充胶层，可以满足小于40μm的窄封装间隙填充要求，还能够较好地避免底部填充时产生气孔，防止无机填料发生沉降，使形成的底部填充胶层具有较高均匀性，从而提高封装可靠性，提高电子元器件服役可靠性，更好地匹配电子封装领域越来越窄、越来越复杂的窄间隙封装应用需求。其中，底部填充胶层可以分散电子元器件表面承载的应力，缓解芯片、焊接凸点和基板三者热膨胀系数CTE不匹配产生的内应力问题，保护焊接凸点，确保电子元器件的可靠运行。
本申请实施方式中，所述无机填料的D10为0.2μm-0.3μm，D50为0.6μm-1.0μm，D90为1.5μm-2.7μm。将无机填料的D10、D50和D90控制在上述特定尺寸范围，有利于树脂组合物在添加较大量小粒径无机填料的情况下仍具有低粘度和高流动性，提升树脂组合物的窄间隙封装填充能力，还能够较好地避免底部填充时产生气孔，防止无机填料发生沉降，使形成的底部填充胶层具有更高的均匀性，从而提高封装可靠性，提高电子元器件服役可靠性。
本申请实施方式中，所述无机填料的粒度分布系数P＝(D90-D10)/D50≤3.5。适合的粒度分布系数控制有利于更好地提升树脂组合物体系的窄间隙封装填充能力。
本申请实施方式中，所述无机填料的比表面积为2m2/g-10m2/g。将无机填料的比表面积控制在适合的范围，可以增强无机填料与环氧树脂的相互作用，更好地防止无机填料沉降，使树脂组合物用于底部填充时形成的底部填充胶层中的无机填料和环氧树脂分布更均匀，从而使得底部填充胶层的性能更均匀，最终有利于提高封装可靠性，提高电子元器件服役可靠性。
本申请实施方式中，所述无机填料包括二氧化硅、氧化铝、氧化镁、氮化铝、氮化硅中的一种或多种。这些无机填料的加入可以降低树脂组合物体系的热膨胀系数降低热应力，还可以降低吸水率、降低成型收缩率、减少树脂溢料、提高机械性能、提高热形变温度和增强耐磨性。
本申请实施方式中，所述无机填料为球形颗粒，球形度大于98％。通过选用球形度较高的球形颗粒无机填料加入树脂组合物中，可以提高树脂组合物的流动性，增强窄间隙填充能力，更好地满足大尺寸芯片的底部填充。
本申请实施方式中，所述树脂组合物中，所述无机填料的质量占比大于或等于55％。通过将无机填料控制在较高的含量，有利于降低树脂组合物固化物的热膨胀系数，降低热应力，从而提高封装可靠性。
本申请实施方式中，所述树脂组合物中，所述无机填料的质量占比为55％-80％。通过将无机填料控制在适合的较高含量范围，能够使得树脂组合物更好地兼顾低热膨胀系数、高玻璃转化温度Tg、低粘度和适合力学性能，从而保证树脂组合物能够作为底部填充材料实现窄间隙的底部填充，提高封装可靠性。
本申请实施方式中，所述环氧树脂包括缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂、缩水甘油胺类环氧树脂、脂肪族环氧树脂、双酚F型环氧树脂、萘型环氧树脂、氨基苯酚型环氧树脂、联萘型环氧树脂、双酚A型环氧树脂、酚醛型环氧树脂中的一种或多种。树脂组合物中，环氧树脂可以是一种，也可以是多种(两种或两种以上)的组合。
由于芯片处理信号越来越多，工作结温也随之升高，特别是在开关设备的时候，瞬时温度会更高，存在芯片结温大于封装材料的玻璃化转变温度Tg的情况，此时封装材料会软化，导致芯片失效。为了更好地提高树脂组合物固化物的玻璃化转变温度Tg，本申请实施方式中，所述环氧树脂包括多官能环氧树脂。多官能(三官能及三官能以上)环氧树脂与固化剂交联，可以提高固化物整体的交联密度，提高树脂组合物固化物的玻璃化转变温度Tg，从而提高封装可靠性，有效避免芯片失效问题的产生，提高高结温芯片的可靠性。
本申请实施方式中，所述固化剂在所述树脂组合物中的质量占比为5％-20％。适合的固化剂含量可使得环氧树脂能够顺利实现固化，获得满足封装的基本物性。
本申请实施方式中，所述环氧树脂在所述树脂组合物中的质量占比为15％-30％。适合的环氧树脂含量可使得树脂组合物能够满足封装的基本物性，实现填充，且能够更好地保证芯片、焊接凸点和基板之间的强结合。
本申请实施方式中，所述固化剂包括胺类固化剂和/或酸酐固化剂。本申请实施方式中，酸酐固化剂可以是六氢苯酐、四氢苯酐、甲基四氢苯酐、甲基六氢苯酐、六氢邻苯二甲酸酐、烷基六氢邻苯二甲酸酐、四氢邻苯二甲酸酐、琥珀酸酐、甲基纳迪克酸酐、氢化甲基那迪克酸酐、5-降冰片烯-2，3-二酸酐、三烷基四氢邻苯二甲酸酐等中的一种或多种。本申请实施方式中，胺类固化剂可以是芳香胺类固化剂，也可以是脂肪胺类固化剂，具体地，胺类固化剂可以是二乙基甲苯二胺、聚醚胺、异佛尔酮二胺、3,3’-二甲基-4,4’-二氨基-二环己基甲烷等。
本申请实施方式中，为了改善树脂组合物的性能，所述树脂组合物还可以包括添加剂，所述添加剂包括偶联剂、增韧剂、应力改性剂、固化促进剂、着色剂、分散剂、离子捕捉剂、消泡剂、流平剂、阻燃剂、脱模剂、流动改进剂中的一种或多种。添加剂可以根据具体需要加入。
本申请实施方式中，所述树脂组合物在110℃的粘度小于0.3Pa.s。树脂组合物具有较低粘度，有利于保证树脂组合物在进行封装填充时具有良好的流动性和填充性，从而较好地满足窄间隙填充需求，提高封装效果。
本申请实施方式中，所述树脂组合物的固化物的玻璃化转变温度大于或等于145℃。树脂组合物在固化后具有较高的玻璃化转变温度Tg，可以提高封装所得胶层的服役可靠性，有效避免芯片失效问题的产生。
本申请实施方式中，所述树脂组合物的固化物的热膨胀系数为25ppm/℃-35ppm/℃。较低的热膨胀系数有利于提升封装可靠性。
本申请实施例第二方面提供一种封装材料，用于电子元器件的密封包装(即封装)，所述封装材料包括本申请实施例第一方面所述的树脂组合物和/或所述树脂组合物的固化物。采用本申请实施例提供的树脂组合物作为封装材料(即电子封装材料)，用于电子元器件的封装，可以提升封装效果，提高电子器件的服役可靠性。
本申请实施例第三方面提供第一方面所述的树脂组合物在电子元器件密封包装中的应用。即树脂组合物作为电子封装材料在电子封装领域的应用。
本申请实施方式中，所述树脂组合物在电子元器件密封包装中的应用可包括所述树脂组合物作为底部 填充材料在电子元器件密封包装中的应用。具体地将树脂组合物填充在基板与电子元器件之间，经加热固化后形成牢固的填充层，可降低电子元器件与基板之间因热膨胀系数差异所造成的应力冲击，提高封装结构的强度和连接可靠性，增强封装结构整体的抗跌落性能。
本申请实施例第四方面提供一种固化物，所述固化物包括本申请实施例第一方面所述的树脂组合物的固化物。本申请实施例的固化物可以是填充在基板与电子元器件之间，具体位于基板与电子元器件连接的焊接凸点之间。
本申请实施例第五方面提供一种封装器件，所述封装器件包括本申请实施例第四方面所述的固化物。本申请实施例封装器件，采用本申请实施例提供的树脂组合物的固化物实现封装，具有较高的服役可靠性。
本申请实施方式中，所述封装器件包括基板、设置在所述基板上的电子元器件，所述电子元器件朝向所述基板的一侧表面设有多个焊接凸点，所述焊接凸点之间设有底部填充胶层，所述底部填充胶层包括所述固化物。本申请实施方式中，所述封装器件还包括覆盖在所述电子元器件表面的塑封体。本申请中，电子元器件包括但不限于芯片，当电子元器件为芯片时，封装器件为一芯片封装结构。
本申请实施例还提供一种终端设备，所述终端设备包括电路板和设置在所述电路板上的本申请实施例第五方面所述的封装器件。本申请实施例终端设备采用本申请实施例提供的封装器件可以提高终端设备的服役可靠性。
本申请实施例还提供一种通信设备，所述通信设备包括本申请实施例第五方面所述的封装器件。
本申请实施例还提供一种通信基站，所述通信基站包括本申请实施例第五方面所述的封装器件。
附图说明
图1为本申请一实施例提供的封装器件100的结构示意图；
图2为本申请实施例封装器件100设置于电路板上的示意图；
图3为本申请实施例提供的终端设备200的结构示意图。
具体实施方式
下面将结合本申请实施例中的附图，对本申请实施例进行说明。
在基板与芯片之间填充封装材料经热固化后形成牢固的底部填充胶层，可降低芯片与基板之间因热膨胀系数差异所造成的应力冲击，保护芯片、基板和焊接凸点，提高封装结构的强度和连接可靠性，提升封装结构整体的抗跌落性能。而目前先进封装结构中为增加I/O数、缩短信号传输距离，封装间隙越来越小(小于40μm)，封装界面愈加复杂，因此要求封装材料具备优异的窄间隙填充能力，更好地匹配电子封装领域越来越窄、越来越复杂的窄间隙封装应用需求。基于此，本申请实施例提供一种树脂组合物，该树脂组合物为液态，是一种液态封装材料，该树脂组合物具有良好的窄间隙封装填充能力。该树脂组合物可以但不限于应用于倒装芯片(Flip chip)、扇入型晶圆级封装FOWLP、扇出型晶圆级封装FOWLP、硅通孔技术TSV、2.5D封装、3D封装、嵌入型晶圆级球栅阵列封装eWLB等先进封装结构中。
本申请实施例提供一种树脂组合物，该树脂组合物包括环氧树脂、固化剂和无机填料，其中，无机填料的截止粒径为3μm，无机填料的D10为0.1μm-0.4μm，D50为0.5μm-1.1μm，D90为1.3μm-2.9μm。
其中，截止粒径即卡断粒径、截断粒径，是理论上的最大粒径，但受工艺限制，无机填料中可能不可避免地存在个别一些超过截止粒径的无机填料颗粒，具体地可能存在ppm量级的大于截止粒径的无机填料颗粒。例如，无机填料的截止粒径为3μm，是指粒径基本都是小于或等于3μm，粒径大于3μm的在ppm量级的无机填料。
本申请实施例提供的树脂组合物在室温下为液态，为液态树脂组合物，具体是一种液态的环氧树脂组合物，该树脂组合物通过选用截止粒径为3μm的无机填料，并将无机填料的D10、D50和D90控制在特定尺寸范围，由于无机填料具有较小的截止粒径，且由于特定粒径分布控制使得树脂组合物在添加较大量小粒径无机填料的情况下仍具有低粘度和高流动性，最终可使得树脂组合物具有良好的窄间隙封装填充能力。将该树脂组合物作为底部填充材料填充于电子元器件(如芯片)、焊接凸点和基板之间形成底部填充胶层，可以满足小于40μm的窄封装间隙填充要求，还能够较好地避免底部填充时产生气孔，防止无机填料发生沉降，使形成的底部填充胶层具有较高均匀性，从而提高封装可靠性，提高电子元器件服役可靠性，更好地匹配电子封装领域越来越窄、越来越复杂的窄间隙封装应用需求。其中，底部填充胶层可以分散电子元器件表面承载的应力，缓解芯片、焊接凸点和基板三者热膨胀系数CTE不匹配产生的内应力问题，保护焊接凸点，确保电子元器件的可靠运行。
本申请实施方式中，无机填料的D10为0.1μm-0.4μm，D50为0.5μm-1.1μm，D90为1.2μm-2.9μm。具体地，D10例如可以是0.1μm、0.2μm、0.3μm、0.4μm，D50例如可以是0.5μm、0.6μm、0.7μm、0.8μm、0.9μm、1.0μm、1.1μm，D90例如可以是1.3μm、1.4μm、1.5μm、1.6μm、1.7μm、1.8μm、1.9μm、2.0μm、2.1μm、2.2μm、2.3μm、2.4μm、2.5μm、2.6μm、2.7μm、2.8μm、2.9μm。一些实施例中，无机填料的D10为0.2μm-0.3μm，D50为0.6μm-1.0μm，D90为1.5μm-2.7μm。D10、D50和D90是累计粒度分布数分别达到10％、50％、90％时所对应的粒径。将无机填料的D10、D50和D90控制在上述特定尺寸范围，有利于树脂组合物在添加较大量小粒径无机填料的情况下仍具有低粘度和高流动性，提升树脂组合物的窄间隙封装填充能力，还能够较好地避免底部填充时产生气孔，防止无机填料发生沉降，使形成的底部填充胶层具有更高的均匀性，从而提高封装可靠性，提高电子元器件服役可靠性。
需要说明的是，受检测方法和仪器限制，本申请实施例无机填料的粒径值可能存在本领域检测方法或检测仪器允许的误差。
本申请实施方式中，无机填料的粒度分布系数P＝(D90-D10)/D50≤3.5。一些实施方式中，无机填料的粒度分布系数P为1-3.5。具体地，无机填料的粒度分布系数P例如可以是1、1.5、2、2.3、2.5、2.7、3、3.5。适合的粒度分布系数控制有利于更好地提升树脂组合物体系的窄间隙封装填充能力。
本申请实施方式中，无机填料的比表面积为2m2/g-10m2/g。比表面积是指单位质量物料所具有的总面积。本申请实施方式中，无机填料的比表面积具体可以是2m2/g、3m2/g、4m2/g、5m2/g、6m2/g、7m2/g、8m2/g、9m2/g、10m2/g。将无机填料的比表面积控制在适合的范围，可以增强无机填料与环氧树脂的相互作用，更好地防止无机填料沉降，使树脂组合物用于底部填充时形成的底部填充胶层中的无机填料和环氧树脂分布更均匀，从而使得底部填充胶层的性能更均匀，最终有利于提高封装可靠性，提高电子元器件服役可靠性。
本申请实施方式中，无机填料可以是包括二氧化硅、氧化铝、氧化镁、氮化铝、氮化硅中的一种或多种。这些无机填料的加入可以降低树脂组合物体系的热膨胀系数降低热应力，还可以降低吸水率、降低成型收缩率、减少树脂溢料、提高机械性能、提高热形变温度和增强耐磨性，从而提升树脂组合物作为封装材料应用的封装可靠性。
本申请实施方式中，无机填料为球形颗粒，球形度大于98％。通过选用球形度较高的球形颗粒无机填料加入树脂组合物中，可以提高树脂组合物的流动性，增强窄间隙填充能力，更好地满足大尺寸芯片的底部填充。
本申请一些实施方式中，无机填料为球形二氧化硅。采用球形二氧化硅有利于更好地提升树脂组合物的流动性和热膨胀系数。
本申请实施方式中，可以通过扫描电子显微镜(scanning electron microscope,SEM))等对无机填料的截止粒径进行测量；可以通过动态光散射粒度分析仪分析无机填料的粒径分布。
本申请实施方式中，树脂组合物中，无机填料的质量占比大于或等于55％。通过将无机填料控制在较高的含量，有利于降低树脂组合物固化物的热膨胀系数，降低热应力，从而提高封装可靠性。
本申请实施方式中，树脂组合物中，无机填料的质量占比为55％-80％。本申请一些实施例中，树脂组合物中，无机填料的质量占比为55％、56％、57％、58％、59％、60％、61％、62％、63％、64％、65％、66％、67％、68％、69％、70％、71％、72％、75％、80％。通过将无机填料控制在适合的较高含量范围，能够使得树脂组合物更好地兼顾低热膨胀系数、高玻璃转化温度Tg、低粘度和适合力学性能，从而保证树脂组合物能够作为底部填充材料实现窄间隙的底部填充，提高封装可靠性。
本申请实施方式中，环氧树脂可以是包括缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂、缩水甘油胺类环氧树脂、脂肪族环氧树脂、双酚F型环氧树脂、萘型环氧树脂、氨基苯酚型环氧树脂、联萘型环氧树脂、双酚A型环氧树脂、酚醛型环氧树脂中的一种或多种。树脂组合物中，环氧树脂可以是一种，也可以是多种(两种或两种以上)的组合。本申请一些实施方式中，环氧树脂包括双酚F型环氧树脂、氨基苯酚环氧树脂、双酚A型环氧树脂、萘系环氧树脂、联萘型环氧树脂中的一种或多种。
本申请实施方式中，可通过核磁共振谱图、红外光谱仪、元素分析等方法分析获知环氧树脂种类和固化剂种类。
由于芯片处理信号越来越多，工作结温也随之升高，特别是在开关设备的时候，瞬时温度会更高，存在芯片结温大于封装材料的玻璃化转变温度Tg的情况，此时封装材料会软化，导致芯片失效。为了更好地提高树脂组合物固化物的玻璃化转变温度Tg，本申请实施方式中，所述环氧树脂包括多官能环氧树脂。多官能(三官能及三官能以上)环氧树脂与固化剂交联，可以提高固化物整体的交联密度，提高树脂组合 物固化物的玻璃化转变温度Tg，从而提高封装可靠性，有效避免芯片失效问题的产生，提高高结温芯片的可靠性。
本申请实施方式中，固化剂在树脂组合物中的质量占比为5％-20％。本申请一些实施例中，固化剂在树脂组合物中的质量占比可以是5％、6％、7％、8％、9％、10％、11％、12％、13％、14％、15％、16％、17％、18％、19％、20％。适合的固化剂含量可使得环氧树脂能够顺利实现固化，获得满足封装的基本物性。
本申请实施方式中，环氧树脂在树脂组合物中的质量占比为15％-30％。本申请一些实施例中，环氧树脂在树脂组合物中的质量占比可以是15％、16％、17％、18％、19％、20％、21％、22％、23％、24％、25％、26％、27％、28％、29％、30％。适合的环氧树脂含量可使得树脂组合物能够满足封装的基本物性，实现填充，且能够更好地保证芯片、焊接凸点和基板之间的强结合。
本申请实施方式中，固化剂可以是包括胺类固化剂和/或酸酐固化剂。本申请实施方式中，酸酐固化剂可以是六氢苯酐、四氢苯酐、甲基四氢苯酐、甲基六氢苯酐、六氢邻苯二甲酸酐、烷基六氢邻苯二甲酸酐、四氢邻苯二甲酸酐、琥珀酸酐、甲基纳迪克酸酐、氢化甲基那迪克酸酐、5-降冰片烯-2，3-二酸酐、三烷基四氢邻苯二甲酸酐等中的一种或多种。本申请实施方式中，胺类固化剂可以是芳香胺类固化剂，也可以是脂肪胺类固化剂，具体地，胺类固化剂可以是二乙基甲苯二胺、聚醚胺、异佛尔酮二胺、3,3’-二甲基-4,4’-二氨基-二环己基甲烷等中的一种或多种。其中，胺类固化剂具有更低的吸水性，有利于降低树脂组合物固化物的吸水率。本申请树脂组合物中，可以是包括一种固化剂，也可以是包括多种(两种或两种以上)固化剂。
本申请实施方式中，为了改善树脂组合物的性能，树脂组合物中还可以包括添加剂，所述添加剂包括但不限于偶联剂、增韧剂、应力改性剂、固化促进剂、着色剂、分散剂、离子捕捉剂、消泡剂、流平剂、阻燃剂、脱模剂、流动改进剂中的一种或多种。添加剂可以根据具体需要加入。本申请实施方式中，对偶联剂、增韧剂、应力改性剂、固化促进剂、着色剂、分散剂、离子捕捉剂、消泡剂、流平剂、阻燃剂、脱模剂、流动改进剂的具体种类无特殊限定。其中，偶联剂包括但不限于γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、3-氨基丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷中的一种或多种。固化促进剂包括但不限于叔胺(例如N,N-二甲基卞胺等)、咪唑、改性咪唑(例如二甲基咪唑、1-苯基二甲基咪唑等)中的一种或多种。
本申请实施方式中，树脂组合物在110℃的粘度小于0.3Pa.s。树脂组合物的粘度可以采用流变仪进行测试。一些实施方式中，树脂组合物在110℃的粘度小于0.25Pa.s。一些实施方式中，树脂组合物在110℃的粘度小于0.2Pa.s。一些实施方式中，树脂组合物在110℃的粘度小于0.15Pa.s。树脂组合物的粘度可以采用流变仪进行测试。需要说明的是，本申请实施例的树脂组合物需要在-40℃及以下低温保存和运输。上述粘度是指树脂组合物刚制备好后测得的粘度，或在解冻后测得的粘度。树脂组合物具有较低粘度，有利于保证树脂组合物在进行封装填充时具有良好的流动性和填充性，从而较好地满足窄间隙填充需求，提高封装效果。
本申请实施方式中，树脂组合物的固化物的玻璃化转变温度大于或等于145℃。本申请一些实施方式中，树脂组合物的固化物的玻璃化转变温度大于或等于150℃。本申请一些实施方式中，树脂组合物的固化物的玻璃化转变温度大于或等于160℃。本申请一些实施方式中，树脂组合物的固化物的玻璃化转变温度大于或等于170℃。本申请一些实施方式中，树脂组合物的固化物的玻璃化转变温度大于或等于180℃。树脂组合物在固化后具有较高的玻璃化转变温度Tg，可以提高封装所得胶层的服役可靠性，有效避免芯片失效问题的产生。
本申请实施方式中，树脂组合物的固化物的热膨胀系数为25ppm/℃-35ppm/℃。具体地，树脂组合物的固化物的热膨胀系数例如可以是25ppm/℃、26ppm/℃、27ppm/℃、28ppm/℃、29ppm/℃、30ppm/℃、31ppm/℃、32ppm/℃、33ppm/℃、34ppm/℃、35ppm/℃。较低的热膨胀系数有利于提升封装可靠性。
本申请实施例的树脂组合物可以是通过将各成分搅拌混合制备得到。搅拌混合可以单独用置顶式机械搅拌器、双行星搅拌机、匀质机、三辊研磨机进行，也可以是将上述装置组合使用。
本申请实施例的树脂组合物是液体封装材料，可以是灌装于10cc、30cc或更大体积的针筒中进行储存。本申请实施例的树脂组合物需要在-40℃及以下低温保存和运输。
本申请实施例的树脂组合物在受热时会发生固化，其中的环氧树脂和固化剂可发生化学反应而形成三维网状聚合物。该树脂组合物在固化后转变成一定形状的固化物，该固化物可以是薄膜状、片状或具有三维立体结构。本申请上述树脂组合物通常为液态。该液态树脂组合物可以直接作为液态胶水，可经涂覆填充、固化后形成胶层。
本申请实施例的树脂组合物为一种含无机填料的环氧树脂组合物，该树脂组合物具有良好的窄间隙封装填充能力。该树脂组合物可以作为底部填充材料填充于电子元器件(如芯片)、焊接凸点和基板之间形成底部填充胶层，可以满足40μm及以下的窄封装间隙填充要求，还能够较好地避免底部填充时产生气孔，防止无机填料发生沉降，使形成的底部填充胶层具有较高均匀性，从而提高封装可靠性，提高电子元器件服役可靠性。该树脂组合物可以用于但不限于应用在倒装芯片(Flip chip)、扇入型晶圆级封装FOWLP、扇出型晶圆级封装FOWLP、硅通孔技术TSV、2.5D封装、3D封装、嵌入型晶圆级球栅阵列封装eWLB等先进封装结构中，采用这些先进封装结构的产品(如处理器等)可用于手机、电脑、汽车等整机设备中。本申请树脂组合物还可以应用于大面积成型、薄型无需研磨封装、无源器件和POP(package-on-package，封装体叠层技术)封装等，这些封装产品可应用于移动电子设备的无线装置和自驱动传感器等设备中。
本申请实施例还提供一种封装材料，该封装材料为电子封装材料，用于电子元器件的密封包装，该封装材料包括本申请实施例上述提供的树脂组合物和/或上述提供的树脂组合物的固化物。采用本申请实施例上述提供的树脂组合物作为封装材料，用于电子元器件的封装，可以提升封装效果，提高电子器件的服役可靠性。
本申请实施例提供上述的树脂组合物在电子封装领域的应用，即树脂组合物作为电子封装材料在电子封装领域的应用。具体地在电子元器件密封包装中的应用。本申请实施例中，电子元器件可以是芯片、晶体管(如二极管、三极管)、LED、阻容感元件(如电阻、电容、电感)等。封装的结构形式可以是倒装芯片(Flip chip)、扇入型晶圆级封装FOWLP、扇出型晶圆级封装FOWLP、硅通孔技术TSV、2.5D封装、3D封装、嵌入型晶圆级球栅阵列封装eWLB等先进封装结构，还可以是大面积成型、薄型无需研磨封装、无源器件封装和POP(package-on-package，封装体叠层技术)封装等封装结构。
本申请实施方式中，树脂组合物在电子元器件密封包装中的应用可包括树脂组合物作为底部填充材料在电子元器件密封包装中的应用。具体地将树脂组合物填充在基板与电子元器件之间，经加热固化后形成牢固的填充层，可降低电子元器件与基板之间因热膨胀系数差异所造成的应力冲击，提高封装结构的强度和连接可靠性，增强封装结构整体的抗跌落性能。
本申请实施例还提供一种固化物，该固化物包括本申请实施例上述的树脂组合物的固化物。本申请实施例的固化物可以是填充在基板与电子元器件之间，具体位于基板与电子元器件连接的焊接凸点之间。固化物可以是薄膜状、片状、三维立体结构等形状，固化物具有低热膨胀系数CTE，高玻璃化转变温度Tg，高机械强度，低吸水性等特性。
请参阅图1，本申请实施例还提供一种封装器件100，图1是本申请一实施方式中封装器件100的结构示意图。该封装器件100可以是电子器件封装件，封装器件100包括本申请实施例上述的树脂组合物的固化物。具体地，封装器件100包括基板10、设置在基板10上的电子元器件20，电子元器件20朝向基板10的一侧表面设有多个焊接凸点30，焊接凸点30之间即基板10、电子元器件20、焊接凸点30之间设有底部填充胶层40，底部填充胶层40包括本申请实施例上述的树脂组合物的固化物。本申请实施方式中，封装器件100还包括覆盖在电子元器件200表面的塑封体60。本申请实施方式中，焊接凸点30通过基板10中的导通结构50与电子元器件20电连接。其中，电子元器件20可以是各种需要封装的元器件，包括但不限于是芯片、晶体管(如二极管、三极管)、LED、阻容感元件(如电阻、电容、电感)等中的一种或多种。当电子元器件20为芯片时，封装器件100为一芯片封装结构。电子元器件20可通过焊接附接至基板10表面，基板10可以是再布线层(RDL)。参见图2，封装器件100可以焊接至电路板101上，基板10远离电子元器件20的一侧可设置多个金属球70，封装器件100中的电子元器件20可通过导通结构50、金属球70与电路板101电连接，基板10与电路板101、金属球70之间设有填充胶层80，该填充胶层80也可以是包括本申请实施例上述的树脂组合物的固化物。
本申请实施例封装器件100采用本申请实施例提供的树脂组合物对电子元器件进行封装，可现实窄间隙填充，工艺操作性高，封装可靠性高。
参见图3，本申请实施例还提供一种终端设备200，终端设备200包括壳体201和设置在壳体201内的电路板和封装器件100，在终端设备200内部，封装器件100可以是如图2所示设置在电路板101上，且与电路板101电连接。终端设备200可以是手机、平板电脑、笔记本电脑、便携机、智能穿戴产品、电视机、录像机、摄录机、收音机、收录机、车载终端、鼠标、键盘、麦克风、扫描仪等产品。
本申请实施例还提供一种通信设备，通信设备包括本申请实施例上述的封装器件100。封装器件100可以是电连接固定于电路板上。通信设备可以是各类有线通信设备或无线通信设备，包括但不限于是通信转换设备、避雷器、天线、网关、遥控器、雷达、对讲机、交换机、路由器等。
本申请实施例还提供一种通信基站，通信基站包括本申请实施例上述的封装器件100。封装器件100可以是电连接固定于电路板上。
下面分多个实施例对本申请实施例进行进一步的说明。
实施例1
一种树脂组合物，包括如下质量占比的各组分：三官能的氨基苯酚环氧树脂26％，芳香胺固化剂二乙基甲苯二胺13％，无机填料A1 60％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.3μm，D50为1.0μm，D90为2.7μm，比表面积为7m2/g的球形二氧化硅。
实施例2
一种树脂组合物，包括如下质量占比的各组分：三官能的氨基苯酚环氧树脂26％，芳香胺固化剂二乙基甲苯二胺13％，无机填料A2 60％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.2μm，D50为0.8μm，D90为2.4μm，比表面积为7.6m2/g的球形二氧化硅。
实施例3
一种树脂组合物，包括如下质量占比的各组分：三官能的氨基苯酚环氧树脂26％，芳香胺固化剂二乙基甲苯二胺13％，无机填料A3 60％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.2μm，D50为0.6μm，D90为2.0μm，比表面积为8m2/g的球形二氧化硅。
实施例4
一种树脂组合物，包括如下质量占比的各组分：三官能的氨基苯酚环氧树脂24.5％，芳香胺固化剂二乙基甲苯二胺9.5％，无机填料A1 65％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.3μm，D50为1.0μm，D90为2.7μm，比表面积为7m2/g的球形二氧化硅。
实施例5
一种树脂组合物，包括如下质量占比的各组分：三官能的氨基苯酚环氧树脂22.5％，芳香胺固化剂二乙基甲苯二胺6.5％，无机填料A1 70％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.3μm，D50为1.0μm，D90为2.7μm，比表面积为7m2/g的球形二氧化硅。
实施例6
一种树脂组合物，包括如下质量占比的各组分：双酚F环氧树脂15％，三官能的氨基苯酚环氧树脂10％，芳香胺固化剂二乙基甲苯二胺9％，无机填料A1 65％，偶联剂γ-缩水甘油醚氧丙基三甲氧基硅烷1％，其中，无机填料为截止粒径为3μm，D10为0.3μm，D50为1.0μm，D90为2.7μm，比表面积为7m2/g的球形二氧化硅。
对比例1
对比例1与实施例1的区别仅在于采用无机填料B1，无机填料为截止粒径为5μm，D10为0.1μm，D50为1.5μm，D90为4.8μm，比表面积为6m2/g的球形二氧化硅。
对比例2
对比例2与实施例1的区别仅在于采用无机填料B2，无机填料为截止粒径为3μm，D10为0.1μm，D50为0.3μm，D90为0.9μm，比表面积为9m2/g的球形二氧化硅。
上述实施例1至实施例6、对比例1和对比例2的配方列于表1。将本申请实施例1至实施例6、对比例1和对比例2制备的树脂组合物进行粘度测试、流动长度测试。将本申请实施例1至实施例6制备的树脂组合物的固化物、对比例1和对比例2的树脂组合物的固化物进行玻璃化转变温度Tg测试。其中，树脂组合物的粘度采用流变仪测定，在110℃，取50rpm下的粘度；树脂组合物的流动长度测试测定在40μm间隙，110℃下10min的流动长度；树脂组合物固化物的玻璃化转变温度Tg采用动态热机械分析仪测试。
表1各实施例与对比例的测试结果汇总

由表1中实施例1至实施例6，以及对比例1和对比例2的结果可知，本申请实施例1至实施例6通过采用截止粒径为3μm，且D10，D50，D90在特定尺寸范围的球形二氧化硅作为填料，制备得到的树脂组合物可以获得低粘度、窄间隙流动长度大于或等于40mm，表明本申请实施例的树脂组合物具有高流动性，具有良好窄间隙填充能力。而对比例1使用的是截止粒径为5μm的二氧化硅作为填料，树脂组合物粘度较高，在窄间隙的流动长度较短，为38mm。对比例2虽然使用的是截止粒径为3μm，但是其D10为0.1μm，D50为0.3μm，D90为0.9μm，树脂组合物粘度较高，在窄间隙的流动长度较短，为30mm。
另外由实施例1至实施例6可知，使用多官能环氧树脂，可以提高树脂组合物体系的玻璃化转变温度Tg；由实施例1至实施例6可知，通过将树脂组合物中无机填料的质量占比控制在适合范围，可以获得低粘度高流动性。
将本申请实施例1至实施例6，以及对比例1和对比例2的树脂组合物用于25mm*25mm尺寸芯片的底部填充。采用超声波扫描表征填充胶层，以及切片后通过扫描电子显微镜观察底部填充胶层，结果显示本申请实施例1至实施例6的树脂组合物可以实现40μm及以下间隙的完全填充，填充效率高，且底部填充胶层无气泡，无填料沉降。而对比例1的树脂组合物填充效率较低，实现完全填充需要比实施例1至实施例6的树脂组合物更长的时间，且底部填充胶层有无机填料的沉降。而对比例2的树脂组合物则根本无法实现完全填充。
应理解，本文中涉及的第一、第二以及各种数字编号仅为描述方便进行的区分，并不用来限制本申请的范围。
本申请中，“和/或”，描述关联对象的关联关系，表示可以存在三种关系，例如，A和/或B，可以表示：单独存在A，同时存在A和B，单独存在B的情况，其中A,B可以是单数或者复数。字符“/”一般表示前后关联对象是一种“或”的关系。
本申请中，“至少一个”是指一个或者多个，“多个”是指两个或两个以上。“以下至少一项(个)”或其类似表达，是指的这些项中的任意组合，包括单项(个)或复数项(个)的任意组合。例如，“a,b,或c中的至少一项(个)”，或，“a,b,和c中的至少一项(个)”，均可以表示：a,b,c,a-b(即a和b),a-c,b-c,或a-b-c，其中a,b,c分别可以是单个，也可以是多个。
以上所述，仅为本申请的具体实施方式，但本申请的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本申请揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本申请的保护范围之内。因此，本申请的保护范围应以权利要求的保护范围为准。

Claims (26)

  1. 一种树脂组合物，其特征在于，所述树脂组合物包括环氧树脂、固化剂和无机填料，所述无机填料的截止粒径为3μm，所述无机填料的D10为0.1μm-0.4μm，D50为0.5μm-1.1μm，D90为1.3μm-2.9μm。
  2. 如权利要求1所述的树脂组合物，其特征在于，所述无机填料的D10为0.2μm-0.3μm，D50为0.6μm-1.0μm，D90为1.5μm-2.7μm。
  3. 如权利要求1所述的树脂组合物，其特征在于，所述无机填料的粒度分布系数P＝(D90-D10)/D50≤3.5。
  4. 如权利要求1-3任一项所述的树脂组合物，其特征在于，所述无机填料的比表面积为2m2/g-10m2/g。
  5. 如权利要求1-4任一项所述的树脂组合物，其特征在于，所述无机填料包括二氧化硅、氧化铝、氧化镁、氮化铝、氮化硅中的一种或多种。
  6. 如权利要求1-5任一项所述的树脂组合物，其特征在于，所述无机填料为球形颗粒，球形度大于98％。
  7. 如权利要求1-6任一项所述的树脂组合物，其特征在于，所述树脂组合物中，所述无机填料的质量占比大于或等于55％。
  8. 如权利要求1-7任一项所述的树脂组合物，其特征在于，所述树脂组合物中，所述无机填料的质量占比为55％-80％。
  9. 如权利要求1-8任一项所述的树脂组合物，其特征在于，所述环氧树脂包括缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂、缩水甘油胺类环氧树脂、脂肪族环氧树脂、双酚F型环氧树脂、萘型环氧树脂、氨基苯酚型环氧树脂、联萘型环氧树脂、双酚A型环氧树脂、酚醛型环氧树脂中的一种或多种。
  10. 如权利要求9所述的树脂组合物，其特征在于，所述环氧树脂包括多官能环氧树脂。
  11. 如权利要求1-10任一项所述的树脂组合物，其特征在于，所述固化剂在所述树脂组合物中的质量占比为5％-20％。
  12. 如权利要求1-11任一项所述的树脂组合物，其特征在于，所述环氧树脂在所述树脂组合物中的质量占比为15％-30％。
  13. 如权利要求1-12任一项所述的树脂组合物，其特征在于，所述固化剂包括胺类固化剂和/或酸酐固化剂。
  14. 如权利要求1-13任一项所述的树脂组合物，其特征在于，所述树脂组合物还包括添加剂，所述添加剂包括偶联剂、增韧剂、应力改性剂、固化促进剂、着色剂、分散剂、离子捕捉剂、消泡剂、流平剂、阻燃剂、脱模剂、流动改进剂中的一种或多种。
  15. 如权利要求1-14任一项所述的树脂组合物，其特征在于，所述树脂组合物在110℃的粘度小于0.3Pa.s。
  16. 如权利要求1-15任一项所述的树脂组合物，其特征在于，所述树脂组合物的固化物的玻璃化转变温度大于或等于145℃。
  17. 如权利要求1-16任一项所述的树脂组合物，其特征在于，所述树脂组合物的固化物的热膨胀系数为25ppm/℃-35ppm/℃。
  18. 一种封装材料，用于电子元器件的密封包装，其特征在于，所述封装材料包括权利要求1-17任一项所述的树脂组合物和/或所述树脂组合物的固化物。
  19. 如权利要求1-17任一项所述的树脂组合物在电子元器件密封包装中的应用。
  20. 如权利要求19所述的应用，其特征在于，所述树脂组合物在电子元器件密封包装中的应用包括所述树脂组合物作为底部填充材料。
  21. 一种固化物，其特征在于，所述固化物包括权利要求1-17任一项所述的树脂组合物的固化物。
  22. 一种封装器件，其特征在于，所述封装器件包括如权利要求21所述的固化物。
  23. 如权利要求22所述的封装器件，其特征在于，所述封装器件包括基板、设置在所述基板上的电子元器件，所述电子元器件朝向所述基板的一侧表面设有多个焊接凸点，所述焊接凸点之间设有底部填充胶层，所述底部填充胶层包括所述固化物。
  24. 一种终端设备，其特征在于，所述终端设备包括电路板和设置在所述电路板上的如权利要求22或23所述的封装器件。
  25. 一种通信设备，其特征在于，所述通信设备包括如权利要求22或23所述的封装器件。
  26. 一种通信基站，其特征在于，所述通信基站包括如权利要求22或23所述的封装器件。
PCT/CN2023/118230 2022-09-15 2023-09-12 树脂组合物及其应用 Ceased WO2024055959A1 (zh)

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