TW201446950A - Resin sheet for electronic device sealing and production method for electronic device package - Google Patents

Resin sheet for electronic device sealing and production method for electronic device package Download PDF

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Publication number
TW201446950A
TW201446950A TW103111072A TW103111072A TW201446950A TW 201446950 A TW201446950 A TW 201446950A TW 103111072 A TW103111072 A TW 103111072A TW 103111072 A TW103111072 A TW 103111072A TW 201446950 A TW201446950 A TW 201446950A
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Taiwan
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resin sheet
resin
electronic component
temperature
sealing
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TW103111072A
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Chinese (zh)
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Eiji Toyoda
yusaku Shimizu
Chie Iino
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Nitto Denko Corp
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    • C—CHEMISTRY; METALLURGY
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of 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
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C08G59/621—Phenols
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    • 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
    • C08G59/68—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 catalysts used
    • C08G59/686—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 catalysts used containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
    • H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
    • H01L21/561—Batch processing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293—Organic, e.g. plastic
    • H01L23/295—Organic, e.g. plastic containing a filler
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/93—Batch processes
    • H01L24/95—Batch processes at chip-level, i.e. with connecting carried out on a plurality of singulated devices, i.e. on diced chips
    • H01L24/97—Batch processes at chip-level, i.e. with connecting carried out on a plurality of singulated devices, i.e. on diced chips the devices being connected to a common substrate, e.g. interposer, said common substrate being separable into individual assemblies after connecting
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • H01L2224/161—Disposition
    • H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
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    • H01L2224/10—Bump connectors; Manufacturing methods related thereto
    • H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
    • H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
    • H01L2224/161—Disposition
    • H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/16245—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • H01L2224/93—Batch processes
    • H01L2224/95—Batch processes at chip-level, i.e. with connecting carried out on a plurality of singulated devices, i.e. on diced chips
    • H01L2224/97—Batch processes at chip-level, i.e. with connecting carried out on a plurality of singulated devices, i.e. on diced chips the devices being connected to a common substrate, e.g. interposer, said common substrate being separable into individual assemblies after connecting
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
    • H01L23/3107—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape the device being completely enclosed
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    • H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/10—Bump connectors ; Manufacturing methods related thereto
    • H01L24/15—Structure, shape, material or disposition of the bump connectors after the connecting process
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  • Epoxy Resins (AREA)
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Abstract

Provided is a resin sheet having excellent storage stability at normal temperature. The present invention pertains to a resin sheet for electronic device sealing in which the exothermic onset temperature measured by differential scanning calorimetry is 120 DEG C or higher and the exothermic peak temperature is 150-200 DEG C.

Description

電子元件密封用樹脂薄片及電子元件封裝體之製造方法 Resin sheet for electronic component sealing and method of manufacturing electronic component package 發明領域 Field of invention

本發明有關於電子元件密封用樹脂薄片及電子元件封裝體之製造方法。 The present invention relates to a resin sheet for electronic component sealing and a method of manufacturing the electronic component package.

發明背景 Background of the invention

在電子元件封裝體之製作上，代表性的做法是採用將已固定於基板等的1個或複數個電子元件以密封樹脂來密封，並依需要將密封體切割，使之成為電子元件單元之封裝體的順序。 In the manufacture of an electronic component package, one or a plurality of electronic components fixed to a substrate or the like are sealed with a sealing resin, and the sealing body is cut as necessary to become an electronic component unit. The order of the packages.

如此的密封樹脂通常是以冷蔵或冷凍來保存。此係因為若以常溫保存，則硬化反應進行徐緩以致品質降低。然而，從提升操作性等的觀點來看，改善常溫保存性是有所需求的。 Such a sealing resin is usually stored by cold or freezing. This is because if the storage is carried out at normal temperature, the hardening reaction proceeds slowly and the quality is lowered. However, from the viewpoint of improving operability and the like, improvement in room temperature preservability is required.

先行技術文獻 Advanced technical literature 專利文獻 Patent literature

專利文獻1：日本特開2013-7028號公報 Patent Document 1: Japanese Laid-Open Patent Publication No. 2013-7028

專利文獻2：日本特開2006-19714號公報 Patent Document 2: Japanese Laid-Open Patent Publication No. 2006-19714

發明概要 Summary of invention

在專利文獻1記載著，將環氧樹脂、無機充填劑及硬化促進劑等捏合來調製捏合物，接著，將捏合物行塑性加工，藉此形成樹脂薄片。然而，在專利文獻1之樹脂薄片的製法下，因捏合時捏合物的溫度上昇，一部分的硬化促進劑會有活性化的情形。一旦硬化促進劑活性化，該硬化促進劑會成為反應起點，以致即便在常溫下亦會慢慢進行硬化反應，因此樹脂薄片的常溫保存性會降低。 Patent Document 1 discloses that an epoxy resin, an inorganic filler, a curing accelerator, and the like are kneaded to prepare a kneaded product, and then the kneaded material is plastically processed to form a resin sheet. However, in the production method of the resin sheet of Patent Document 1, a part of the hardening accelerator may be activated by the temperature rise of the kneaded compound at the time of kneading. When the hardening accelerator is activated, the hardening accelerator becomes a starting point of the reaction, so that the curing reaction proceeds slowly even at normal temperature, and the room temperature preservability of the resin sheet is lowered.

又，在專利文獻2記載著，將含有溶劑、環氧樹脂及硬化促進劑等的清漆塗布在薄膜上，接著，使塗布膜乾燥，藉此形成樹脂薄片。然而，在專利文獻2樹脂薄片的製法(溶劑塗裝)下，硬化促進劑容易與環氧樹脂等融合，因此硬化促進劑會變成容易反應的狀態，一部分的硬化促進劑會有活性化的情形。 Further, Patent Document 2 discloses that a varnish containing a solvent, an epoxy resin, a curing accelerator, and the like is applied onto a film, and then the coating film is dried to form a resin sheet. However, in the production method (solvent coating) of the resin sheet of Patent Document 2, since the curing accelerator is easily fused with an epoxy resin or the like, the curing accelerator becomes in a state of being easily reacted, and a part of the curing accelerator is activated. .

本發明以解決前述課題，並提供常溫保存性優異的樹脂薄片為目的。 In order to solve the above problems, the present invention has an object of providing a resin sheet excellent in room temperature preservability.

本發明有關於一種電子元件密封用樹脂薄片，其利用示差掃描熱析儀測定的發熱起始溫度為120℃以上，且發熱波峰溫度為150~200℃。 The present invention relates to a resin sheet for sealing an electronic component, which has a heat generation starting temperature of 120 ° C or more and a heat generation peak temperature of 150 to 200 ° C measured by a differential scanning calorimeter.

本發明電子元件密封用樹脂薄片因為滿足如此特性，在常溫下實質上不會進行硬化反應。因此，常溫保存性是優異的。 Since the resin sheet for electronic component sealing of the present invention satisfies such characteristics, it does not substantially undergo a hardening reaction at normal temperature. Therefore, the room temperature preservability is excellent.

利用前述示差掃描熱析儀測定的DSC曲線中，相對於發熱波峰面積整體，在發熱波峰溫度±30℃之溫度範圍中的面積宜為70%以上。因為是70%以上，DSC曲線在高溫域會形成陡峭的發熱波峰。亦即，在常溫下實質上不會進行硬化反應，則常溫保存性是優異的。 In the DSC curve measured by the above-described differential scanning calorimeter, the area in the temperature range of the heat generation peak temperature of ±30 ° C is preferably 70% or more with respect to the entire heat generation peak area. Because it is more than 70%, the DSC curve will form a steep heat peak in the high temperature range. That is, since the hardening reaction does not substantially occur at normal temperature, the room temperature preservability is excellent.

在25℃的條件下保存4週後的最低熔融黏度宜為保存前之最低熔融黏度的2倍以下。因為是2倍以下，可良好地抑制在常溫下的硬化反應，則常溫保存性是優異的。 The minimum melt viscosity after storage for 4 weeks at 25 ° C is preferably less than 2 times the lowest melt viscosity before storage. Since it is 2 times or less, the hardening reaction at normal temperature can be satisfactorily suppressed, and the room temperature preservability is excellent.

前述電子元件密封用樹脂薄片中之填充物的含量宜為70~90體積%。 The content of the filler in the resin sheet for electronic component sealing is preferably 70 to 90% by volume.

前述電子元件密封用樹脂薄片，宜為將環氧樹脂、酚樹脂、熱塑性樹脂、填充物及硬化促進劑捏合而獲得捏合物，並對該捏合物塑性加工成薄片狀所得者。若藉上述，相較於溶劑塗裝法，硬化促進劑難以與環氧樹脂等融合，硬化促進劑會較難以反應，因而可改善常溫保存性。 The resin sheet for electronic component sealing is preferably obtained by kneading an epoxy resin, a phenol resin, a thermoplastic resin, a filler, and a curing accelerator to obtain a kneaded product, and plastically processing the kneaded product into a sheet shape. According to the above, compared with the solvent coating method, the hardening accelerator is difficult to be fused with an epoxy resin or the like, and the hardening accelerator is more difficult to react, so that the room temperature preservability can be improved.

前述硬化促進劑宜為咪唑系硬化促進劑。且前述咪唑系硬化促進劑宜為潛伏性硬化促進劑。 The hardening accelerator is preferably an imidazole-based hardening accelerator. Further, the imidazole-based hardening accelerator is preferably a latent curing accelerator.

本發明又有關於一種電子元件封裝體的製造方法，其包含下述步驟：積層步驟，係以覆蓋1個或複數個電子元件的方式將前述電子元件密封用樹脂薄片積層在前述電子元件上；及密封體形成步驟，係使前述電子元件密封用樹脂薄片硬化來形成密封體。 The present invention relates to a method of manufacturing an electronic component package, comprising the steps of: laminating a resin sheet for sealing an electronic component on the electronic component so as to cover one or a plurality of electronic components; And a sealing body forming step of curing the resin sheet for electronic component sealing to form a sealed body.

11‧‧‧樹脂薄片 11‧‧‧Resin sheet

11a‧‧‧支持體 11a‧‧‧Support

12‧‧‧印刷配線基板 12‧‧‧Printed wiring substrate

13‧‧‧SAW濾波器 13‧‧‧SAW filter

13a‧‧‧突起電極 13a‧‧‧protruding electrode

14‧‧‧中空部分 14‧‧‧ hollow part

15‧‧‧密封體 15‧‧‧ Sealing body

18‧‧‧電子元件封裝 18‧‧‧Electronic component packaging

圖1為示意性顯示關於本發明一種實施形態之樹 脂薄片的剖面圖。 Figure 1 is a schematic diagram showing a tree relating to an embodiment of the present invention A cross-sectional view of a lipid sheet.

圖2A為示意性顯示關於本發明一種實施形態之電子元件封裝體製造方法之一步驟的圖。 Fig. 2A is a view schematically showing a step of a method of manufacturing an electronic component package according to an embodiment of the present invention.

圖2B為示意性顯示關於本發明一種實施形態之電子元件封裝體製造方法之一步驟的圖。 Fig. 2B is a view schematically showing a step of a method of manufacturing an electronic component package according to an embodiment of the present invention.

圖2C為示意性顯示關於本發明一種實施形態之電子元件封裝體製造方法之一步驟的圖。 Fig. 2C is a view schematically showing a step of a method of manufacturing an electronic component package according to an embodiment of the present invention.

用以實施發明的型態 Type used to implement the invention

以下將舉實施形態來詳細說明本發明，但本發明並非僅以該等實施形態為限。 The present invention will be described in detail below with reference to the embodiments, but the present invention is not limited to these embodiments.

[電子元件密封用樹脂薄片] [Resin sheet for electronic component sealing]

圖1為示意性顯示關於本發明一種實施形態之樹脂薄片11的剖面圖。典型上，樹脂薄片11是以積層在聚對苯二甲酸乙二酯(PET)薄膜等支持體11a上的狀態來提供。此外，為易於剝離樹脂薄片11，可在支持體11a施行脫模處理。 Fig. 1 is a cross-sectional view schematically showing a resin sheet 11 according to an embodiment of the present invention. Typically, the resin sheet 11 is provided in a state of being laminated on a support 11a such as a polyethylene terephthalate (PET) film. Further, in order to facilitate the peeling of the resin sheet 11, a release treatment can be performed on the support 11a.

利用示差掃描熱析儀(DSC)測定，樹脂薄片11的發熱起始溫度是120℃以上，且發熱波峰溫度是150~200℃。 The heat generation onset temperature of the resin sheet 11 was 120 ° C or higher and the heat generation peak temperature was 150 to 200 ° C as measured by a differential scanning calorimeter (DSC).

因為發熱起始溫度是120℃以上，且發熱波峰溫度是150~200℃，則在常溫下實質上不會進行硬化反應。因此，樹脂薄片11之常溫保存性是優異的。 Since the heat generation starting temperature is 120 ° C or more and the heat generation peak temperature is 150 to 200 ° C, the hardening reaction is not substantially performed at normal temperature. Therefore, the room temperature preservability of the resin sheet 11 is excellent.

發熱起始溫度的上限並無特別限定，但從樹脂薄片的製造成本、製造效率的觀點來看，例如，是170℃以下。 The upper limit of the heat generation starting temperature is not particularly limited, but is, for example, 170 ° C or less from the viewpoint of the production cost of the resin sheet and the production efficiency.

發熱波峰溫度宜為160℃以上，又宜為190℃以下。 The peak temperature of the heat generation is preferably 160 ° C or more, and preferably 190 ° C or less.

發熱起始溫度及發熱波峰溫度可用實施例記載的方法來測定。 The heat generation onset temperature and the heat generation peak temperature can be measured by the method described in the examples.

發熱起始溫度及發熱波峰溫度可藉由硬化促進劑的種類來控制。 The heat initiation temperature and the heat generation peak temperature can be controlled by the type of the hardening accelerator.

在利用示差掃描熱析儀測定的DSC曲線中，相對於發熱波峰面積整體，在發熱波峰溫度±30℃之溫度範圍中的面積宜為70%以上，且以80%以上較佳。若在70%以上，則DSC曲線在高溫域會形成陡峭的發熱波峰。亦即，在常溫下實質上不會進行硬化反應，則樹脂薄片11的常溫保存性是優異的。 In the DSC curve measured by the differential scanning calorimeter, the area in the temperature range of the heat generation peak temperature of ±30 ° C is preferably 70% or more with respect to the entire heat generation peak area, and is preferably 80% or more. If it is above 70%, the DSC curve will form a steep heat peak in the high temperature range. In other words, the resin sheet 11 is excellent in normal temperature preservability when the curing reaction is not substantially performed at normal temperature.

在25℃的條件下保存4週後的最低熔融黏度宜為保存前最低熔融黏度的2倍以下，且以1.5倍以下為佳。若在2倍以下，可良好地抑制在常溫下的硬化反應，則常溫保存性是優異的。 The minimum melt viscosity after storage for 4 weeks at 25 ° C is preferably less than 2 times the minimum melt viscosity before storage, and preferably 1.5 times or less. When it is 2 times or less, the hardening reaction at normal temperature can be satisfactorily suppressed, and the room temperature preservability is excellent.

此外，最低熔融黏度可用實施例記載的方法來測定。 Further, the lowest melt viscosity can be measured by the method described in the examples.

保存前的最低熔融黏度並無特別限定，然通常為20~20000Pa．s，且宜為3000~10000Pa．s。 The minimum melt viscosity before storage is not particularly limited, but is usually 20 to 20000 Pa. s, and should be 3000~10000Pa. s.

樹脂薄片11的製造方法並無特別限定，但宜為將環氧樹脂、酚樹脂、熱塑性樹脂、填充物及硬化促進劑捏合而獲得捏合物，並將該捏合物塑性加工成薄片狀的方法。若藉由上述，相較於溶劑塗裝法，硬化促進劑難以與環氧樹脂等融合，硬化促進劑會較難以反應，因此可改善 常溫保存性。 The method for producing the resin sheet 11 is not particularly limited, but a method in which an epoxy resin, a phenol resin, a thermoplastic resin, a filler, and a curing accelerator are kneaded to obtain a kneaded product, and the kneaded product is plastically processed into a sheet shape is preferable. According to the above, compared with the solvent coating method, the hardening accelerator is difficult to be fused with an epoxy resin or the like, and the hardening accelerator is more difficult to react, and thus can be improved. Storeability at room temperature.

具體上係將環氧樹脂、酚樹脂、熱塑性樹脂、填充物及硬化促進劑以混合輥、加壓式捏揉機、擠出機等習知的捏合機來熔融捏合，藉此調製捏合物，並將獲得之捏合物塑性加工成薄片狀。在捏合條件方面，溫度的上限宜為140℃以下、且以130℃以下為佳。因為是140℃以下，可抑制硬化促進劑在樹脂薄片製作過程中活性化，而可獲得良好的常溫保存性。溫度的下限宜為上述各成分之軟化點以上，例如30℃以上，且宜為50℃以上。 Specifically, the epoxy resin, the phenol resin, the thermoplastic resin, the filler, and the hardening accelerator are melt-kneaded by a conventional kneading machine such as a mixing roll, a pressure kneader, or an extruder, thereby preparing a kneaded product, and The obtained kneaded material was plastically processed into a flake shape. In terms of kneading conditions, the upper limit of the temperature is preferably 140 ° C or lower, and preferably 130 ° C or lower. Since it is 140 ° C or less, the hardening accelerator can be inhibited from being activated during the production of the resin sheet, and good room temperature preservability can be obtained. The lower limit of the temperature is preferably at least the softening point of each of the above components, for example, 30 ° C or higher, and preferably 50 ° C or higher.

在環氧樹脂方面並無特別限定者。例如可使用三苯甲烷型環氧樹脂、甲酚酚醛型環氧樹脂、聯苯型環氧樹脂、改質雙酚A型環氧樹脂、雙酚A型環氧樹脂、雙酚F型環氧樹脂、改質雙酚F型環氧樹脂、二環戊二烯型環氧樹脂、苯酚酚醛型環氧樹脂、苯氧基樹脂等各種的環氧樹脂。該等環氧樹脂可單獨使用、亦可2種以上併用。 There is no particular limitation on the epoxy resin. For example, a triphenylmethane type epoxy resin, a cresol novolac type epoxy resin, a biphenyl type epoxy resin, a modified bisphenol A type epoxy resin, a bisphenol A type epoxy resin, a bisphenol F type epoxy resin can be used. Various epoxy resins such as a resin, a modified bisphenol F-type epoxy resin, a dicyclopentadiene type epoxy resin, a phenol novolak type epoxy resin, and a phenoxy resin. These epoxy resins may be used singly or in combination of two or more.

從確保環氧樹脂硬化後之靭性及環氧樹脂之反應性的觀點來看，宜為環氧基當量為150~250、軟化點或融點為50~130℃之在常溫下為固態者，其中，從可靠性的觀點來看，以三苯甲烷型環氧樹脂、甲酚酚醛型環氧樹脂、聯苯型環氧樹脂為佳。 From the viewpoint of ensuring the toughness after curing of the epoxy resin and the reactivity of the epoxy resin, it is preferably an epoxy group having an epoxy equivalent of 150 to 250, a softening point or a melting point of 50 to 130 ° C, which is solid at normal temperature. Among them, from the viewpoint of reliability, a triphenylmethane type epoxy resin, a cresol novolac type epoxy resin, and a biphenyl type epoxy resin are preferred.

酚樹脂只要是與環氧樹脂之間會發生硬化反應者，即無特別限定。可使用例如苯酚酚醛樹脂、苯酚芳烷基樹脂、聯苯芳烷基樹脂、二環戊二烯型酚樹脂、甲酚酚醛樹脂、可溶酚醛樹脂等。該等酚樹脂可單獨使用，亦可2 種以上併用。 The phenol resin is not particularly limited as long as it undergoes a hardening reaction with the epoxy resin. For example, a phenol novolak resin, a phenol aralkyl resin, a biphenyl aralkyl resin, a dicyclopentadiene type phenol resin, a cresol novolak resin, a resol resin, or the like can be used. These phenolic resins can be used alone or as 2 More than one kind.

作為酚樹脂，從與環氧樹脂之反應性的觀點來看，宜使用羥基當量是70~250、且軟化點為50~110℃者，於此之中，從硬化反應性高的觀點來看，可適宜使用苯酚酚醛樹脂。又，從可靠性的觀點來看，可適宜使用如苯酚芳烷基樹脂或聯苯芳烷基樹脂之類低吸濕性者。 As the phenol resin, from the viewpoint of reactivity with an epoxy resin, it is preferred to use a hydroxyl group equivalent of 70 to 250 and a softening point of 50 to 110 ° C. From the viewpoint of high curing reactivity, A phenol novolac resin can be suitably used. Further, from the viewpoint of reliability, a low hygroscopicity such as a phenol aralkyl resin or a biphenyl aralkyl resin can be suitably used.

在熱塑性樹脂方面，可舉天然橡膠、丁基橡膠、異戊二烯橡膠、氯平橡膠、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物、聚丁二烯樹脂、聚碳酸酯樹脂、熱塑性聚醯亞胺樹脂、6-尼龍或6,6-尼龍等的聚醯胺樹脂；苯氧基樹脂、丙烯酸樹脂、PBT或PET等的飽和聚酯樹脂；聚醯胺醯亞胺樹脂、氟樹脂、苯乙烯-異丁烯-苯乙烯嵌段共聚物、甲基丙烯酸甲酯-丁二烯-苯乙烯共聚物(MBS樹脂)等。該等熱塑性樹脂可以單獨、或2種以上併用來使用。於此之中，從低應力性、低吸水性的觀點來看，宜為苯乙烯-異丁烯-苯乙烯嵌段共聚物。又，從與環氧樹脂或酚樹脂等的摩擦較小、可在穩定的溫度條件(比較低溫的條件)下捏合的理由來看，宜為MBS樹脂。 Examples of the thermoplastic resin include natural rubber, butyl rubber, isoprene rubber, chloroprene rubber, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, ethylene-acrylate copolymer, and polybutadiene resin. Polycarbonate resin, polycarbonate resin, thermoplastic polyimide resin, 6-nylon or 6,6-nylon; saturated polyester resin such as phenoxy resin, acrylic resin, PBT or PET; polydecylamine A quinone imine resin, a fluororesin, a styrene-isobutylene-styrene block copolymer, a methyl methacrylate-butadiene-styrene copolymer (MBS resin), or the like. These thermoplastic resins may be used singly or in combination of two or more kinds. Among them, from the viewpoint of low stress and low water absorption, a styrene-isobutylene-styrene block copolymer is preferred. Further, from the viewpoint of less friction with an epoxy resin or a phenol resin or the like and kneading under stable temperature conditions (lower temperature conditions), it is preferably an MBS resin.

熱塑性樹脂的平均粒徑並無特別限定，但宜使用較小者，例如5~500μm，且宜為50~200μm。藉此，可以在穩定的溫度條件(比較低溫的條件)下捏合。 The average particle diameter of the thermoplastic resin is not particularly limited, but it is preferably used in a smaller amount, for example, 5 to 500 μm, and preferably 50 to 200 μm. Thereby, it is possible to knead under stable temperature conditions (lower temperature conditions).

此外，平均粒徑，例如可藉由下述方法導出：使用從母群任意提取的試料，並使用雷射繞射散射式粒度分布測 定裝置來測定。 Further, the average particle diameter can be derived, for example, by using a sample arbitrarily extracted from a parent group and using a laser diffraction scattering type particle size distribution measurement. Determine the device to measure.

在填充物方面並無特別限定，但宜為無機充填材。作為無機充填材，可舉例如石英玻璃、滑石、二氧化矽(熔融二氧化矽或結晶性二氧化矽)、氧化鋁、氮化鋁、氮化矽、氮化硼等。於此之中，從可良好地降低線膨張係數的理由來看，宜為二氧化矽、氧化鋁，且以二氧化矽為佳。在二氧化矽方面，從流動性優異的理由來看，宜為熔融二氧化矽，且以球狀熔融二氧化矽為佳。 The filler is not particularly limited, but is preferably an inorganic filler. Examples of the inorganic filler include quartz glass, talc, cerium oxide (melted cerium oxide or crystalline cerium oxide), aluminum oxide, aluminum nitride, tantalum nitride, and boron nitride. Among them, from the standpoint that the linear expansion coefficient can be favorably lowered, it is preferably cerium oxide or aluminum oxide, and cerium oxide is preferred. In the case of cerium oxide, from the viewpoint of excellent fluidity, it is preferred to melt cerium oxide, and it is preferable to melt cerium dioxide in a spherical shape.

填充物的平均粒徑宜為1μm以上，且以5μm以上為佳。若為1μm以上，則容易獲得樹脂薄片的可撓性、柔軟性。填充物的平均粒徑宜為40μm以下，且以30μm以下為佳。若為40μm以下，則容易使填充物高度填充率化。 The average particle diameter of the filler is preferably 1 μm or more, and more preferably 5 μm or more. When it is 1 μm or more, flexibility and flexibility of the resin sheet are easily obtained. The average particle diameter of the filler is preferably 40 μm or less, and preferably 30 μm or less. When it is 40 μm or less, it is easy to increase the filling rate.

此外，平均粒徑，例如可藉由下述方法導出：使用從母群任意提取的試料，並使用雷射繞射散射式粒度分布測定裝置來測定。 Further, the average particle diameter can be derived, for example, by using a sample arbitrarily extracted from a parent group and measuring it using a laser diffraction scattering type particle size distribution measuring apparatus.

填充物宜為利用矽烷偶合劑處理過(前處理)者。藉此，可提升與樹脂的濕潤性，並可以在穩定的溫度條件(比較低溫的條件)下捏合。 The filler is preferably treated with a decane coupling agent (pretreatment). Thereby, the wettability with the resin can be improved, and the kneading can be performed under stable temperature conditions (lower temperature conditions).

矽烷偶合劑為分子中具有水解性基及有機官能基的化合物。 The decane coupling agent is a compound having a hydrolyzable group and an organic functional group in the molecule.

在水解性基方面，可舉例如甲氧基、乙氧基等的碳數為1~6的烷氧基；乙醯氧基、2-甲氧基乙氧基等。於此之中，從容易除去因水解產生之醇等揮發成分的理由來看，宜為甲氧基。 Examples of the hydrolyzable group include an alkoxy group having 1 to 6 carbon atoms such as a methoxy group or an ethoxy group; an ethoxy group, a 2-methoxyethoxy group, and the like. Among these, a methoxy group is preferable from the viewpoint of easily removing a volatile component such as an alcohol generated by hydrolysis.

在有機官能基方面，可舉乙烯基、環氧基、苯乙烯基、甲基丙烯醯基、丙烯醯基、胺基、脲基、巰基、硫醚基、異氰酸酯基等。於此之中，從容易與環氧樹脂、酚樹脂反應的理由來看，宜為環氧基。 Examples of the organic functional group include a vinyl group, an epoxy group, a styryl group, a methacryloyl group, an acryloyl group, an amine group, a urea group, a fluorenyl group, a thioether group, an isocyanate group, and the like. Among them, from the viewpoint of easy reaction with an epoxy resin or a phenol resin, an epoxy group is preferred.

在矽烷偶合劑方面，可舉例如乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷等含有乙烯基的矽烷偶合劑；2-(3,4-環氧基環己基)乙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二乙氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷等含有環氧基的矽烷偶合劑；對苯乙烯基三甲氧基矽烷等含有苯乙烯基的矽烷偶合劑；3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷等含有甲基丙烯酸基的矽烷偶合劑；3-丙烯醯氧基丙基三甲氧基矽烷等含有丙烯醯基的矽烷偶合劑；N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-三乙氧基甲矽烷基-N-(1,3-二甲基-亞丁基)丙基胺、N-苯基-3-胺基丙基三甲氧基矽烷、N-(乙烯基苄基)-2-胺基乙基-3-胺基丙基三甲氧基矽烷等含有胺基的矽烷偶合劑；3-脲基丙基三乙氧基矽烷等的含有脲基的矽烷偶合劑；3-巰基丙基甲基二甲氧基矽烷、3-巰基丙基三甲氧基矽烷等含有巰基的矽烷偶合劑；四硫化雙(三乙氧基甲矽烷基丙基)等 含有硫化基的矽烷偶合劑；3-異氰酸酯基丙基三乙氧基矽烷等含有異氰酸酯基的矽烷偶合劑等。 Examples of the decane coupling agent include a vinyl group-containing decane coupling agent such as vinyltrimethoxydecane or vinyltriethoxysilane; 2-(3,4-epoxycyclohexyl)ethyltrimethoxy group; Decane, 3-glycidoxypropylmethyldimethoxydecane, 3-glycidoxypropyltrimethoxydecane, 3-glycidoxypropylmethyldiethoxydecane, a cyclodecane coupling agent containing an epoxy group such as 3-glycidoxypropyltriethoxydecane; a decyl coupling agent containing a styryl group such as a styryltrimethoxydecane; and a 3-methylpropenyloxy group; Propylmethyldimethoxydecane, 3-methylpropenyloxypropyltrimethoxydecane, 3-methylpropenyloxypropylmethyldiethoxydecane, 3-methylpropene oxime a decane coupling agent containing a methacryl group, such as a propyl triethoxy decane; a decane coupling agent containing an acrylonitrile group such as 3-propenyloxypropyltrimethoxydecane; N-2-(aminoethyl) --3-aminopropylmethyldimethoxydecane, N-2-(aminoethyl)-3-aminopropyltrimethoxydecane, 3-aminopropyltrimethoxydecane, 3 -aminopropyltriethoxy Decane, 3-triethoxycarbamido-N-(1,3-dimethyl-butylene)propylamine, N-phenyl-3-aminopropyltrimethoxydecane, N-(ethylene Amino group-containing decane coupling agent such as benzyl-2-ylethyl-3-aminopropyltrimethoxy decane; ureido-containing decane coupling such as 3-ureidopropyltriethoxy decane Mixture; decane-containing decane coupling agent such as 3-mercaptopropylmethyldimethoxydecane, 3-mercaptopropyltrimethoxydecane; tetrasulfide bis(triethoxycarbamylpropyl) a decane coupling agent containing a sulfurized group; a decane coupling agent containing an isocyanate group, such as 3-isocyanate propyl triethoxy decane.

作為利用矽烷偶合劑來處理填充物的方法並無特別限定，可舉在溶劑中混合填充物與矽烷偶合劑的濕式法、在氣相中處理填充物與矽烷偶合劑的乾式法等。 The method for treating the filler by the decane coupling agent is not particularly limited, and examples thereof include a wet method in which a filler and a decane coupling agent are mixed in a solvent, a dry method in which a filler and a decane coupling agent are treated in a gas phase, and the like.

矽烷偶合劑的處理量並無特別限定，但宜相對於未處理的填充物100重量份，以矽烷偶合劑0.1~1重量份來處理。 The treatment amount of the decane coupling agent is not particularly limited, but it is preferably treated with 0.1 to 1 part by weight of the decane coupling agent per 100 parts by weight of the untreated filler.

在硬化促進劑方面，若為可使環氧樹脂與酚樹脂之硬化進行者則無特別限定，可舉例如四苯基鏻四苯基硼酸(商品名：TPP-K)、四苯基鏻四-對-三硼酸(商品名：TPP-MK)、三苯基膦三苯基硼烷(商品名：TPP-S)等的磷-硼素系硬化促進劑(皆為北興化學工業(股)製)。 In the case of curing the epoxy resin and the phenol resin, the curing accelerator is not particularly limited, and examples thereof include tetraphenylphosphonium tetraphenylboronic acid (trade name: TPP-K) and tetraphenylphosphonium tetrachloride. Phosphorus-boron-based hardening accelerators such as p-triboric acid (trade name: TPP-MK) and triphenylphosphine triphenylborane (trade name: TPP-S) (all manufactured by Beixing Chemical Industry Co., Ltd.) ).

又，可舉2-甲基咪唑(商品名：2MZ)、2-十一基咪唑(商品名：C11-Z)、2-十七基咪唑(商品名：C17Z)、1,2-二甲基咪唑(商品名：1.2DMZ)、2-乙基-4-甲基咪唑(商品名：2E4MZ)、2-苯基咪唑(商品名：2PZ)、2-苯基-4-甲基咪唑(商品名：2P4MZ)、1-苄基-2-甲基咪唑(商品名：1B2MZ)、1-苄基-2-苯基咪唑(商品名：1B2PZ)、1-氰乙基-2-甲基咪唑(商品名：2MZ-CN)、1-氰乙基-2-十一基咪唑(商品名：C11Z-CN)、偏苯三酸1-氰乙基-2-苯基咪唑酯(商品名：2PZCNS-PW)、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三氮苯(商品名：2MZ-A)、2,4-二胺基-6-[2’-十一基咪唑基-(1’)]-乙基-s-三氮苯(商品名：C11Z-A)、2,4-二胺基-6-[2’- 乙基-4’-甲基咪唑基-(1’)]-乙基-s-三氮苯(商品名：2E4MZ-A)、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三氮苯異氰脲酸加成物(商品名：2MA-OK)、2-苯基-4,5-二羥基甲基咪唑(商品名：2PHZ-PW)、2-苯基-4-甲基-5-羥基甲基咪唑(商品名：2P4MHZ-PW)等的咪唑系硬化促進劑(皆為四國化成工業(股)製)。 Further, 2-methylimidazole (trade name: 2MZ), 2-undecylimidazole (trade name: C11-Z), 2-heptadecylimidazole (trade name: C17Z), 1,2-dimethyl Imidazole (trade name: 1.2DMZ), 2-ethyl-4-methylimidazole (trade name: 2E4MZ), 2-phenylimidazole (trade name: 2PZ), 2-phenyl-4-methylimidazole (trade name: 2PZ) Product name: 2P4MZ), 1-benzyl-2-methylimidazole (trade name: 1B2MZ), 1-benzyl-2-phenylimidazole (trade name: 1B2PZ), 1-cyanoethyl-2-methyl Imidazole (trade name: 2MZ-CN), 1-cyanoethyl-2-undecylimidazole (trade name: C11Z-CN), trimellitic acid 1-cyanoethyl-2-phenylimidazolium ester (trade name) : 2PZCNS-PW), 2,4-diamino-6-[2'-methylimidazolyl-(1')]-ethyl-s-triazobenzene (trade name: 2MZ-A), 2, 4-Diamino-6-[2'-undecidamidazolyl-(1')]-ethyl-s-triazobenzene (trade name: C11Z-A), 2,4-diamino-6 -[2'- Ethyl-4'-methylimidazolyl-(1')]-ethyl-s-triazobenzene (trade name: 2E4MZ-A), 2,4-diamino-6-[2'-methyl Imidazolyl-(1')]-ethyl-s-triazophenyl isocyanurate adduct (trade name: 2MA-OK), 2-phenyl-4,5-dihydroxymethylimidazole (trade name) : 2PHZ-PW), an imidazole-based hardening accelerator such as 2-phenyl-4-methyl-5-hydroxymethylimidazole (trade name: 2P4MHZ-PW) (all manufactured by Shikoku Chemical Industries Co., Ltd.).

又，在咪唑系硬化促進劑方面，亦可舉由5-硝基間苯二甲酸及以式(1)表示之咪唑化合物所構成的包合錯合物、由5-硝基間苯二甲酸及以式(2)表示之咪唑化合物所構成的包合錯合物、由5-硝基間苯二甲酸及以式(3)表示之咪唑化合物所構成的包合錯合物。 Further, in the case of the imidazole-based hardening accelerator, an inclusion complex composed of 5-nitroisophthalic acid and an imidazole compound represented by the formula (1), and 5-nitroisophthalic acid may be used. And an inclusion complex of the imidazole compound represented by the formula (2), an inclusion complex composed of 5-nitroisophthalic acid and an imidazole compound represented by the formula (3).

[化3] [Chemical 3]

所謂包合錯合物，是說客化合物(以式(1)~(3)表示的咪唑化合物)被包合(納入)於主化合物(5-硝基間苯二甲酸)而產生的複合物。然後，本說明書中所謂的主化合物，是利用共價鍵以外(化學鍵結以外)之結合之分子間作用力與客化合物結合而形成化合物者，亦指如上述化合物中形成包合晶格的化合物。又所謂包合晶格，是說主化合物彼此利用共價鍵以外的結合來結合，並在已結合之主化合物其2分子以上空間(間隙)中，利用共價鍵以外之結合(分子間作用力)而包合有客化合物的化合物。 The inclusion complex is a complex produced by a guest compound (an imidazole compound represented by the formulas (1) to (3)) which is encapsulated (incorporated) with a main compound (5-nitroisophthalic acid). . Then, the main compound referred to in the present specification is a compound which forms a compound by binding to a guest compound by an intermolecular force of a bond other than a covalent bond (other than a chemical bond), and also means a compound which forms an inclusion lattice in the above compound. . In addition, the inclusion of a crystal lattice means that the main compounds are bonded to each other by a combination other than a covalent bond, and in a space (gap) of two or more molecules to which the main compound has been bonded, a combination other than a covalent bond is utilized (intermolecular interaction) A compound that contains a guest compound.

此等包合錯合物，是在主化合物之5-硝基間苯二甲酸中，將客化合物之以式(1)~(3)表示之咪唑化合物利用非化學鍵結之分子間作用力等的物理作用力來包合。因此，此等包合錯合物在常溫下並不會起了作為硬化促進劑之作用，但在高溫下因脫離包合，便會活性化為硬化促進劑。 These inclusion complexes are in the intermolecular force of the non-chemical bond of the imidazole compound represented by the formula (1) to (3) in the 5-nitroisophthalic acid of the main compound. The physical force to cover. Therefore, these inclusion complexes do not function as a hardening accelerator at normal temperature, but they are activated as a hardening accelerator by decoupling at a high temperature.

包合錯合物，例如可按如下所述來製作。亦即，可利用將5-硝基間苯二甲酸與選自於由以式(1)~(3)表示之咪唑化合物所構成群組中之至少一者添加於溶劑後，邊適當攪拌，邊進行加熱處理或加熱回流處理，使目標包 合錯合物析出來製作。 The inclusion of the complex compound can be produced, for example, as follows. In other words, at least one selected from the group consisting of the imidazole compounds represented by the formulas (1) to (3) may be added to the solvent, and then stirred. Heat treatment or heat reflow treatment to make the target package The compound is precipitated and produced.

此外，考慮到易對溶劑溶解的情形，宜將5-硝基間苯二甲酸及以式(1)~(3)表示之咪唑化合物分別各自溶解在溶劑後，再混合該等溶解液。在溶劑方面，可使用例如水、甲醇、乙醇、乙酸乙酯、乙酸甲酯、二乙醚、二甲醚、丙酮、甲基乙基酮、乙腈等。 Further, in consideration of the ease of dissolution of the solvent, it is preferred to dissolve the 5-nitroisophthalic acid and the imidazole compound represented by the formulas (1) to (3) in a solvent, and then mix the solutions. As the solvent, for example, water, methanol, ethanol, ethyl acetate, methyl acetate, diethyl ether, dimethyl ether, acetone, methyl ethyl ketone, acetonitrile or the like can be used.

又，在製造包合錯合物時，在5-硝基間苯二甲酸及以式(1)~(3)表示之咪唑化合物的添加比例方面，例如相對於5-硝基間苯二甲酸(主化合物)1莫耳，宜將以式(1)~(3)表示之咪唑化合物(客化合物)設定為0.1~5.0莫耳之比例，且以設定為0.5~3.0莫耳之比例為佳。 Further, in the production of the inclusion complex, the ratio of addition of 5-nitroisophthalic acid and the imidazole compound represented by the formulas (1) to (3), for example, relative to 5-nitroisophthalic acid (Main compound) 1 mole, it is preferred to set the imidazole compound (guest compound) represented by formulas (1) to (3) to a ratio of 0.1 to 5.0 moles, and preferably set to a ratio of 0.5 to 3.0 moles. .

作為製造包合錯合物時的加熱條件，只要為可獲得目標之包合錯合物的溫度範圍即可，例如宜為在40~120℃的範圍下加熱，且以在50~90℃的範圍下加熱為佳。 The heating condition in the case of producing the inclusion complex compound may be a temperature range in which the target inclusion complex is obtained, and for example, it is preferably heated in the range of 40 to 120 ° C and at 50 to 90 ° C. Heating under the range is preferred.

製造包合錯合物時的加熱，宜一邊攪拌含有5-硝基間苯二甲酸與以式(1)~(3)表示之咪唑化合物之溶液或懸浮液一邊進行，且以加熱回流為佳。 The heating in the preparation of the inclusion complex is preferably carried out while stirring a solution or suspension containing 5-nitroisophthalic acid and the imidazole compound represented by the formulas (1) to (3), and heating is preferably carried out. .

熱處理或加熱回流處理後，例如可藉由將溶液或懸浮液在室溫下放置一晚使包合錯合物析出後，再過濾並乾燥來獲得目標之包合錯合物。 After the heat treatment or the heating and reflux treatment, for example, the inclusion complex can be precipitated by leaving the solution or suspension at room temperature overnight, followed by filtration and drying to obtain the target inclusion complex.

在咪唑系硬化促進劑之中，從即便在捏合溫度下亦難以活性化的理由來看，宜為潛伏性的硬化促進劑，且以2-苯基-4,5-二羥基甲基咪唑、由5-硝基間苯二甲酸與 以式(1)表示之咪唑化合物所構成的包合錯合物、由5-硝基間苯二甲酸與以式(2)表示之咪唑化合物所構成的包合錯合物、由5-硝基間苯二甲酸與以式(3)表示之咪唑化合物所構成的包合錯合物為佳。 Among the imidazole-based hardening accelerators, from the viewpoint of difficulty in activation even at the kneading temperature, a latent curing accelerator is preferred, and 2-phenyl-4,5-dihydroxymethylimidazole is used. From 5-nitroisophthalic acid with An inclusion complex of the imidazole compound represented by the formula (1), an inclusion complex composed of 5-nitroisophthalic acid and an imidazole compound represented by the formula (2), and 5-nitrate The inclusion complex of the isophthalic acid and the imidazole compound represented by the formula (3) is preferred.

環氧樹脂、酚樹脂、熱塑性樹脂、填充物及硬化促進劑宜與阻燃劑成分、顏料、矽烷偶合劑等同時捏合。 The epoxy resin, the phenol resin, the thermoplastic resin, the filler, and the hardening accelerator are preferably kneaded together with the flame retardant component, the pigment, the decane coupling agent, and the like.

在阻燃劑成分方面，可使用例如氫氧化鋁、氫氧化鎂、氫氧化鐵、氫氧化鈣、氫氧化錫、錯合化金屬氫氧化物等的各種金屬氫氧化物；偶磷氮化合物等。於此之中，從阻燃性、硬化後之強度優異的理由來看，宜為偶磷氮化合物。 As the flame retardant component, various metal hydroxides such as aluminum hydroxide, magnesium hydroxide, iron hydroxide, calcium hydroxide, tin hydroxide, and a mixed metal hydroxide can be used; an even phosphorus nitrogen compound or the like can be used. . Among them, from the viewpoint of excellent flame retardancy and strength after curing, it is preferably an azo-phosphorus compound.

在顏料方面並無特別限定，可舉碳黑等。 The pigment is not particularly limited, and examples thereof include carbon black.

捏合的時間宜為1分鐘以上，且以5分鐘以上為佳。又，捏合的時間宜為30分鐘以下，且以15分以下為佳。 The kneading time is preferably 1 minute or longer, and preferably 5 minutes or more. Further, the kneading time is preferably 30 minutes or less, and preferably 15 minutes or less.

捏合宜在減壓條件下(減壓環境下)進行。減壓條件下的壓力宜為0.1kg/cm2以下，且以0.05kg/cm2以下為佳。減壓下的壓力下限並無特別限定，但例如為1×10-4kg/cm2以上。 Kneading is preferably carried out under reduced pressure (under reduced pressure). The pressure under reduced pressure is preferably 0.1 kg/cm 2 or less, and preferably 0.05 kg/cm 2 or less. The lower limit of the pressure under reduced pressure is not particularly limited, but is, for example, 1 × 10 -4 kg / cm 2 or more.

熔融捏合後的捏合物，宜不冷卻而直接在高溫狀態下來塑性加工。在塑性加工方法方面並無特別限制，可舉平板壓法、T型擠出法、螺旋型擠出法、輥壓延法、輥捏合法、充氣擠出法、共擠出法、壓光成型法等。在塑 性加工溫度方面，宜為上述各成分的軟化點以上，若考慮到環氧樹脂的熱硬化性及成形性，則為例如40~150℃，且以50~140℃為宜、70~120℃更佳。 The kneaded product after melt-kneading is preferably subjected to plastic working directly at a high temperature without cooling. The plastic working method is not particularly limited, and examples thereof include a flat plate pressing method, a T-type extrusion method, a spiral extrusion method, a roll calendering method, a roll kneading method, a pneumatic extrusion method, a co-extrusion method, and a calender molding method. Wait. In plastic The processing temperature is preferably at least the softening point of each of the above components, and considering the thermosetting property and moldability of the epoxy resin, for example, 40 to 150 ° C, and preferably 50 to 140 ° C, 70 to 120 ° C. Better.

樹脂薄片11的厚度並無特別限定，但宜為100μm以上，且以150μm以上為佳。又，樹脂薄片11的厚度宜為2000μm以下，且以1000μm以下為佳。若為上述範圍內，則可良好地將電子元件密封。 The thickness of the resin sheet 11 is not particularly limited, but is preferably 100 μm or more, and more preferably 150 μm or more. Further, the thickness of the resin sheet 11 is preferably 2000 μm or less, and preferably 1000 μm or less. If it is in the above range, the electronic component can be satisfactorily sealed.

樹脂薄片11可為單層構造，亦可為積層有2層以上樹脂薄片之多層構造，但從無層間剝離之虞、薄片厚度均一性高的理由來看，宜為單層構造。 The resin sheet 11 may have a single-layer structure or a multilayer structure in which two or more layers of resin sheets are laminated. However, it is preferable to have a single-layer structure from the viewpoint of no peeling between layers and high uniformity of thickness of the sheet.

接著，針對樹脂薄片11的組成做說明。 Next, the composition of the resin sheet 11 will be described.

樹脂薄片11中的環氧樹脂及酚樹脂的合計含量宜為2.0重量%以上，且以3.0重量%以上為佳。若為2.0重量%以上，則可獲得對電子元件、基板等良好的接著力。樹脂薄片11中的環氧樹脂及酚樹脂的合計含量，宜為20重量%以下，且以10重量%以下為佳。若為20重量%以下，則可將吸濕性抑制得較低。 The total content of the epoxy resin and the phenol resin in the resin sheet 11 is preferably 2.0% by weight or more, and more preferably 3.0% by weight or more. When it is 2.0% by weight or more, good adhesion to an electronic component, a substrate, or the like can be obtained. The total content of the epoxy resin and the phenol resin in the resin sheet 11 is preferably 20% by weight or less, and preferably 10% by weight or less. When it is 20% by weight or less, the hygroscopicity can be suppressed to be low.

環氧樹脂與酚樹脂的摻合比例，從硬化反應性的觀點來看，宜相對於環氧樹脂中的環氧基1當量，以使酚樹脂中羥基的合計成為0.7~1.5當量的方式來摻合酚樹脂，且以0.9~1.2當量為佳。 The blending ratio of the epoxy resin and the phenol resin is preferably from 1 to 1.5 equivalents based on the epoxy group in the epoxy resin, so that the total amount of the hydroxyl groups in the phenol resin is 0.7 to 1.5 equivalents. The phenol resin is blended and preferably 0.9 to 1.2 equivalents.

樹脂薄片11中之熱塑性樹脂的含量宜為1.0重量%以上，且以1.5重量%以上為佳。若為1.0重量%以上，則可在穩定的溫度條件(比較低溫的條件)下捏合。樹脂薄片 11中之熱塑性樹脂的含量宜為3.5重量%以下，且以3重量%以下為佳。若為3.5重量%以下，則可獲得對電子元件、基板等良好的接著力。 The content of the thermoplastic resin in the resin sheet 11 is preferably 1.0% by weight or more, and more preferably 1.5% by weight or more. When it is 1.0% by weight or more, it can be kneaded under stable temperature conditions (lower temperature conditions). Resin sheet The content of the thermoplastic resin in 11 is preferably 3.5% by weight or less, and preferably 3% by weight or less. When it is 3.5% by weight or less, good adhesion to an electronic component, a substrate, or the like can be obtained.

樹脂薄片11中之填充物的含量宜為70體積%以上，且以74體積%以上為佳。若為70體積%以上，則可將線膨張係數設計得較低。另一方面，填充物的含量宜為90體積%以下，且以85體積%以下為佳。若為90體積%以下，則可獲得良好的柔軟性、流動性、接著性。 The content of the filler in the resin sheet 11 is preferably 70% by volume or more, and more preferably 74% by volume or more. If it is 70% by volume or more, the linear expansion coefficient can be designed to be low. On the other hand, the content of the filler is preferably 90% by volume or less, and preferably 85% by volume or less. When it is 90 vol% or less, good flexibility, fluidity, and adhesion can be obtained.

填充物的含量亦可以「重量%」作為單位來說明。典型上，針對二氧化矽的含量係以「重量%」為單位來說明。 The content of the filler can also be described in terms of "% by weight". Typically, the content of cerium oxide is described in terms of "% by weight".

二氧化矽通常比重為2.2g/cm3，因此二氧化矽含量(重量%)的適宜範圍例如為下者。 The cerium oxide usually has a specific gravity of 2.2 g/cm 3 , and thus a suitable range of the cerium oxide content (% by weight) is, for example, the following.

即，樹脂薄片11中之二氧化矽的含量宜為81重量%以上，且以84重量%以上為佳。樹脂薄片11中之二氧化矽的含量宜為94重量%以下，且以91重量%以下為佳。 That is, the content of cerium oxide in the resin sheet 11 is preferably 81% by weight or more, and preferably 84% by weight or more. The content of cerium oxide in the resin sheet 11 is preferably 94% by weight or less, and preferably 91% by weight or less.

氧化鋁通常比重為3.9g/cm3，因此氧化鋁含量(重量%)的適宜範圍例如為下者。 The alumina generally has a specific gravity of 3.9 g/cm 3 , and thus a suitable range of the alumina content (% by weight) is, for example, the following.

即，樹脂薄片11中之氧化鋁的含量宜為88重量%以上，且以90重量%以上為佳。樹脂薄片11中之氧化鋁的含量宜為97重量%以下。且以95重量%以下為佳。 That is, the content of the alumina in the resin sheet 11 is preferably 88% by weight or more, and more preferably 90% by weight or more. The content of the alumina in the resin sheet 11 is preferably 97% by weight or less. It is preferably 95% by weight or less.

相對於環氧樹脂及酚樹脂的合計100重量份，硬化促進劑的含量宜為0.1重量部以上，且以1重量份以上為佳、為3重量份以上更佳。若為0.1重量份以上，則會在可 行的時間內來完成硬化。又，硬化促進劑的含量宜為15重量份以下，且以10重量份以下為佳、為8重量份以下更佳。若為15重量份以下，則硬化物的強度良好。 The content of the curing accelerator is preferably 0.1 part by weight or more, more preferably 1 part by weight or more, more preferably 3 parts by weight or more, based on 100 parts by weight of the total of the epoxy resin and the phenol resin. If it is 0.1 part by weight or more, it will be The time to complete the hardening. Further, the content of the curing accelerator is preferably 15 parts by weight or less, more preferably 10 parts by weight or less, still more preferably 8 parts by weight or less. When it is 15 parts by weight or less, the strength of the cured product is good.

在有機成分(除去填充物的總成分)100重量%中，阻燃劑成分的含量宜為10重量%以上，且以15重量%以上為佳。若為10重量%以上，則可獲得良好的阻燃性。阻燃劑成分的含量宜為30重量%以下，且以25重量%以下為佳。若為30重量%以下，則硬化物之物性降低(具體而言，玻璃轉化溫度或高溫樹脂強度等物性之降低)會有減少的傾向。 The content of the flame retardant component is preferably 10% by weight or more, and preferably 15% by weight or more, based on 100% by weight of the organic component (total component of the filler). When it is 10% by weight or more, good flame retardancy can be obtained. The content of the flame retardant component is preferably 30% by weight or less, and preferably 25% by weight or less. When it is 30% by weight or less, the physical properties of the cured product are lowered (specifically, the physical properties such as the glass transition temperature or the high-temperature resin strength are lowered).

樹脂薄片11中之顏料的含量宜為0.1~2重量%。 The content of the pigment in the resin sheet 11 is preferably from 0.1 to 2% by weight.

樹脂薄片11可使用在SAW(Surface Acoustic Wave)濾波器；壓力感測器；振動感測器等的MEMS(Micro Electro Mechanical Systems)；LSI等的IC(積體電路)、電晶體等的半導體；電容器；電阻等的電子元件之密封。於此之中，可適宜使用在中空密封為必要之電子元件(具體來說為SAW濾波器、MEMS)的密封，且特別適宜使用在SAW濾波器的密封。 The resin sheet 11 can be used as a semiconductor such as a SAW (Surface Acoustic Wave) filter, a pressure sensor, a MEMS (Micro Electro Mechanical Systems) such as a vibration sensor, an IC (integrated circuit) such as an LSI, or a transistor; Capacitor; sealing of electronic components such as resistors. Among them, a seal for an electronic component (specifically, a SAW filter, MEMS) which is necessary for a hollow seal can be suitably used, and a seal for a SAW filter is particularly suitably used.

在密封方法方面並無特別限定，可舉例如以覆蓋基板上之電子元件的方式將未硬化的樹脂薄片11積層在基板上，接著使樹脂薄片11硬化來密封的方法等。在基板方面並無特別限定，可舉例如印刷配線基板、陶瓷基板、矽基板、金屬基板等。 The sealing method is not particularly limited, and for example, a method in which an uncured resin sheet 11 is laminated on a substrate so as to cover the electronic component on the substrate, and then the resin sheet 11 is cured and sealed. The substrate is not particularly limited, and examples thereof include a printed wiring board, a ceramic substrate, a tantalum substrate, and a metal substrate.

[電子元件封裝體的製造方法] [Method of Manufacturing Electronic Component Package]

圖2A~2C分別是示意性顯示關於本發明一種實施形態電子元件封裝體製造方法之一步驟的圖。在本實施形態，是將搭載在印刷配線基板12上之SAW濾波器13藉由樹脂薄片11來中空密封而製作電子元件封裝體。 2A to 2C are views each schematically showing a step of a method of manufacturing an electronic component package according to an embodiment of the present invention. In the present embodiment, the SAW filter 13 mounted on the printed wiring board 12 is sealed by the resin sheet 11 to form an electronic component package.

(SAW濾波器搭載基板準備步驟) (SAW filter mounting substrate preparation step)

SAW濾波器搭載基板準備步驟，是準備搭載有複數個SAW濾波器13的印刷配線基板12(參考圖2A)。SAW濾波器13可藉由習知方法將形成有預定之梳形電極的壓電晶體切割作成單片化而形成。可使用倒裝晶片接合器或晶粒接合器等習知的裝置將SAW濾波器13搭載於印刷配線基板12上。SAW濾波器13與印刷配線基板12是藉由突塊等的突起電極13a形成電性連結。又，在SAW濾波器13與印刷配線基板12之間，為了不阻礙表面彈性波在SAW濾波器表面的傳播，便維持著中空部分14。SAW濾波器13與印刷配線基板12之間的距離可適宜設定，一般為15~50μm左右。 The SAW filter mounting substrate preparation step is to prepare a printed wiring board 12 on which a plurality of SAW filters 13 are mounted (see FIG. 2A). The SAW filter 13 can be formed by dicing a piezoelectric crystal formed with a predetermined comb-shaped electrode into a single piece by a conventional method. The SAW filter 13 can be mounted on the printed wiring board 12 by a conventional device such as a flip chip bonder or a die bonder. The SAW filter 13 and the printed wiring board 12 are electrically connected by the bump electrodes 13a such as bumps. Further, the hollow portion 14 is maintained between the SAW filter 13 and the printed wiring board 12 so as not to hinder the propagation of the surface acoustic wave on the surface of the SAW filter. The distance between the SAW filter 13 and the printed wiring board 12 can be appropriately set, and is generally about 15 to 50 μm.

(密封步驟) (sealing step)

在密封步驟，是以覆蓋SAW濾波器13的方式對印刷配線基板12積層樹脂薄片11，並將SAW濾波器13以樹脂薄片11來樹脂密封(參考圖2B)。樹脂薄片11之作用是作為密封樹脂，用以從外界保護SAW濾波器13及附屬於其的要素。 In the sealing step, the resin sheet 11 is laminated on the printed wiring substrate 12 so as to cover the SAW filter 13, and the SAW filter 13 is resin-sealed with the resin sheet 11 (refer to FIG. 2B). The resin sheet 11 functions as a sealing resin for protecting the SAW filter 13 and the elements attached thereto from the outside.

將樹脂薄片11積層在印刷配線基板12上的方法並無特別限定，可利用熱壓或積層機等習知的方法來進行。作為熱壓條件，溫度例如為40~100℃，且宜為50~90℃；壓力例如為0.1~10MPa，且宜為0.5~8MPa；時間例如 為0.3~10分鐘，且宜為0.5~5分鐘間。又，若考慮到提升樹脂薄片11對SAW濾波13及印刷配線基板12的密著性及追隨性，宜在減壓條件下(例如0.1~5kPa)行加壓。 The method of laminating the resin sheet 11 on the printed wiring board 12 is not particularly limited, and it can be carried out by a conventional method such as a hot press or a laminator. As a hot pressing condition, the temperature is, for example, 40 to 100 ° C, and preferably 50 to 90 ° C; the pressure is, for example, 0.1 to 10 MPa, and preferably 0.5 to 8 MPa; It is 0.3 to 10 minutes, and preferably 0.5 to 5 minutes. Moreover, in consideration of the adhesion and followability of the lift resin sheet 11 to the SAW filter 13 and the printed wiring board 12, it is preferable to pressurize under a reduced pressure condition (for example, 0.1 to 5 kPa).

(密封體形成步驟) (sealing body forming step)

在密封體形成步驟，是將樹脂薄片11行熱硬化處理來形成密封體15(參考圖2B)。 In the sealing body forming step, the resin sheet 11 is thermally hardened to form a sealing body 15 (refer to FIG. 2B).

作為熱硬化處理的條件，加熱溫度宜為100℃以上，且以120℃以上為佳。另一方面，加熱溫度的上限宜為200℃以下，且以180℃以下為佳。加熱時間宜為10分鐘以上，且以30分以上為佳。另一方面，加熱時間的上限宜為180分鐘以下，且以120分以下為佳。又，亦可依需要來加壓，且宜為0.1MPa以上、以0.5MPa以上為佳。另一方面，上限宜為10MPa以下，且以5MPa以下為佳。 As a condition of the heat hardening treatment, the heating temperature is preferably 100 ° C or more, and preferably 120 ° C or more. On the other hand, the upper limit of the heating temperature is preferably 200 ° C or lower, and preferably 180 ° C or lower. The heating time is preferably 10 minutes or more, and preferably 30 minutes or more. On the other hand, the upper limit of the heating time is preferably 180 minutes or less, and preferably 120 minutes or less. Further, it may be pressurized as needed, and is preferably 0.1 MPa or more and 0.5 MPa or more. On the other hand, the upper limit is preferably 10 MPa or less, and preferably 5 MPa or less.

(切割步驟) (cutting step)

接下來，亦可進行密封體15的切割(參考圖2C)。藉此，可以獲得以SAW濾波器13為單元的電子元件封裝體18。 Next, the sealing of the sealing body 15 can also be performed (refer to FIG. 2C). Thereby, the electronic component package 18 in which the SAW filter 13 is a unit can be obtained.

(基板安裝步驟) (substrate mounting step)

依需要可進行基板安裝步驟，其係對電子元件封裝體18形成再配線及突塊，並將其安裝在另外之基板(圖無顯示)。在對基板安裝電子元件封裝體18時，可使用倒裝晶片接合器或晶粒接合器等的習知的裝置。 The substrate mounting step can be performed as needed, and the electronic component package 18 is formed with rewiring and bumps, and mounted on another substrate (not shown). When the electronic component package 18 is mounted on the substrate, a conventional device such as a flip chip bonder or a die bonder can be used.

實施例 Example

以下舉本發明之適當實施例來詳細說明。但該 實施例記載之材料或摻合量等，在無特別限定性的記載之下，並不會將本發明的範圍僅限定在該等所揭。 The following is a detailed description of suitable embodiments of the invention. But that The materials, blending amounts, and the like described in the examples are not intended to limit the scope of the invention to those disclosed herein.

說明關於使用在實施例的成分。 The ingredients used in the examples are explained.

環氧樹脂：新日鐵化學(股)製的YSLV-80XY(雙酚F型環氧樹脂、環氧當量200g/eq.軟化點80℃) Epoxy resin: YSLV-80XY made of Nippon Steel Chemical Co., Ltd. (bisphenol F type epoxy resin, epoxy equivalent 200g/eq. softening point 80 °C)

酚樹脂：明和化成社製的MEH-7851-SS(具有聯苯基芳烷基骨架的酚樹脂，羥基當量203g/eq.軟化點67℃) Phenol resin: MEH-7851-SS (a phenol resin having a biphenyl aralkyl skeleton, hydroxyl equivalent: 203 g/eq. softening point: 67 ° C) manufactured by Minghe Chemical Co., Ltd.

熱塑性樹脂：三菱麗陽社製METABLEN C-132E(MBS樹脂，平均粒徑120μm) Thermoplastic resin: METABLEN C-132E (MBS resin, average particle size 120μm) manufactured by Mitsubishi Rayon Co., Ltd.

填充物：電氣化學工業社製的FB-9454FC(熔融球状二氧化矽，平均粒子徑20μm) Filler: FB-9454FC (melt spherical cerium oxide, average particle diameter 20 μm) manufactured by Denki Kogyo Co., Ltd.

矽烷偶合劑：信越化學社製的KBM-403(3-環氧丙氧基丙基三甲氧基矽烷) Decane coupling agent: KBM-403 (3-glycidoxypropyltrimethoxydecane) manufactured by Shin-Etsu Chemical Co., Ltd.

矽烷偶合劑處理填充物：將電氣化學工業社製的FB-9454FC(熔融球狀二氧化矽，平均初級粒子徑20μm)以信越化學社製的KBM-403(3-環氧丙氧基丙基三甲氧基矽烷)處理過者(相對於87.9重量份的FB-9454FC，以0.5重量份比例的KBM-403來處理) 矽 偶 偶 : : : : : : : : : : FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB FB Trimethoxydecane treated (relative to 87.9 parts by weight of FB-9454FC, treated with 0.5 parts by weight of KBM-403)

碳黑：三菱化學社製的#20 Carbon black: #20 from Mitsubishi Chemical Corporation

阻燃劑：伏見製藥所製的FP-100(偶磷氮化合物) Flame retardant: FP-100 (Azo Phosphorus Compound) manufactured by Fushimi Pharmaceutical Co., Ltd.

硬化促進劑1：四國化成工業社製的2PHZ-PW(2-苯基-4,5-二羥基甲基咪唑) Hardening accelerator 1: 2PHZ-PW (2-phenyl-4,5-dihydroxymethylimidazole) manufactured by Shikoku Chemicals Co., Ltd.

硬化促進劑2(包合錯合物)：由5-硝基間苯二甲酸與以式(1)表示之2-乙基-4-甲基咪唑所構成的包合錯合物 Hardening accelerator 2 (inclusion complex): an inclusion complex composed of 5-nitroisophthalic acid and 2-ethyl-4-methylimidazole represented by formula (1)

硬化促進劑3(包合錯合物)：由5-硝基間苯二甲酸與以式(2)表示之2-苯基-4,5-二羥基甲基咪唑所構成的包合錯合物 Hardening accelerator 3 (inclusion complex): a mixture of 5-nitroisophthalic acid and 2-phenyl-4,5-dihydroxymethylimidazole represented by formula (2) Object

硬化促進劑4(包合錯合物)：由5-硝基間苯二甲酸與以式(3)表示之2-苯基-4-甲基-5-羥基甲基咪唑所構成的包合錯合物 Hardening accelerator 4 (inclusion complex): inclusion of 5-nitroisophthalic acid and 2-phenyl-4-methyl-5-hydroxymethylimidazole represented by formula (3) Complex

硬化促進劑5：北興化學工業社製的TPP(三苯基膦) Hardening accelerator 5: TPP (triphenylphosphine) manufactured by Behind Chemical Industry Co., Ltd.

硬化促進劑6：四國化成工業社製的2E4MZ(2-乙基-4-甲基咪唑) Hardening accelerator 6: 2E4MZ (2-ethyl-4-methylimidazole) manufactured by Shikoku Chemicals Co., Ltd.

實施例及比較例 Examples and comparative examples

遵照表1記載之摻合比來摻合各成分，並利用輥捏合機在60~120℃、10分鐘、減壓條件下(0.01kg/cm2)熔融捏合來調製捏合物。接著，將獲得之捏合物利用平板加壓法形成薄片狀來製作厚度200μm的樹脂薄片。 Each component was blended in accordance with the blending ratios shown in Table 1, and kneaded by melt kneading at 60 to 120 ° C for 10 minutes under reduced pressure (0.01 kg/cm 2 ). Next, the obtained kneaded material was formed into a sheet shape by a flat plate pressing method to prepare a resin sheet having a thickness of 200 μm.

使用獲得之樹脂薄片(未硬化物)進行下述的評價。結果顯示在表1。 The following evaluation was performed using the obtained resin sheet (unhardened material). The results are shown in Table 1.

[發熱起始溫度及發熱波峰溫度] [Fever start temperature and heat peak temperature]

將樹脂薄片沖切成直徑4mm的圓形來製作樣品。針對此樣品，使用示差掃描熱析儀(TA Instrument製、DSC Q2000)，使之以10℃/分從-50℃升溫至300℃，並描繪DSC曲線，從已描繪的DSC曲線讀取發熱起始溫度及發熱波峰溫度。此外，以發熱曲線之2次微分值成為0的溫度在發熱曲線畫出切線，並讀取與基準線之交點的溫度，將此作為發熱起始溫度。 A sample was prepared by punching a resin sheet into a circular shape having a diameter of 4 mm. For this sample, a differential scanning calorimeter (manufactured by TA Instrument, DSC Q2000) was used, and the temperature was raised from -50 ° C to 300 ° C at 10 ° C / min, and the DSC curve was drawn, and the heat was read from the drawn DSC curve. Starting temperature and heating peak temperature. Further, a temperature at which the second-order differential value of the heat generation curve becomes 0 is plotted on the heat generation curve, and the temperature at the intersection with the reference line is read, and this is taken as the heat generation start temperature.

[發熱波峰溫度±30℃之發熱量的比例] [The ratio of the calorific value of the peak temperature of ±30 °C]

從已描繪的DSC曲線求出於發熱波峰溫度±30℃之溫度範圍中的面積(面積A)，與發熱波峰面積總體(面積B)。然後，利用下述式，算出在發熱波峰溫度±30℃之中的發熱量的比例。 The area (area A) in the temperature range of ±30 ° C of the heat generation peak temperature and the total area of the heat generation peak area (area B) were obtained from the drawn DSC curve. Then, the ratio of the amount of heat generation in the heat generation peak temperature ± 30 ° C was calculated by the following formula.

發熱波峰溫度±30℃之發熱量的比例(%)=面積A/面積B×100。 The ratio (%) of the calorific value of the calorific peak temperature ± 30 ° C = area A / area B × 100.

[保存前的最低熔融黏度] [Minimum melt viscosity before storage]

使用動態黏彈性測定裝置(TA Instruments社製、ARES)來測定樹脂薄片的最低熔融黏度(測定條件：間隙1mm、平行板直徑8mm、測定頻率0.1Hz、以10℃/min升溫至50℃~150℃來測定)。 The lowest melt viscosity of the resin sheet was measured using a dynamic viscoelasticity measuring apparatus (manufactured by TA Instruments, ARES) (measurement conditions: gap 1 mm, parallel plate diameter 8 mm, measurement frequency 0.1 Hz, and temperature increase to 50 ° C to 150 at 10 ° C / min °C to determine).

[保存後的最低熔融黏度] [Minimum melt viscosity after storage]

針對在25℃下保存4週後的樹脂薄片，以與保存前同樣的方法來測定最低熔融黏度。 The lowest melt viscosity was measured in the same manner as before storage for the resin sheet stored at 25 ° C for 4 weeks.

發熱起始溫度為120℃以上、且發熱波峰溫度為150~200℃之實施例1~5的樹脂薄片，其常溫保存前後的最低熔融黏度變化小，在常溫保存性上是優異的。另一方面，發熱起始溫度小於120℃之比較例1、2的樹脂薄片，在常溫保存中硬化反應會進行完畢，無法測定最低熔融黏度。 The resin sheets of Examples 1 to 5 having a heat generation starting temperature of 120 ° C or higher and a heat generation peak temperature of 150 to 200 ° C have a small change in minimum melt viscosity before and after storage at room temperature, and are excellent in storage stability at room temperature. On the other hand, in the resin sheets of Comparative Examples 1 and 2 having a heat generation starting temperature of less than 120 ° C, the curing reaction was completed during the storage at room temperature, and the lowest melt viscosity could not be measured.

又，藉由使用經矽烷偶合劑處理之填充物來代替未處理的填充物，可抑制保存前後之最低熔融黏度的變化(實施例5)。 Further, by using a filler treated with a decane coupling agent instead of the untreated filler, the change in the lowest melt viscosity before and after storage can be suppressed (Example 5).

11‧‧‧樹脂薄片 11‧‧‧Resin sheet

11a‧‧‧支持體 11a‧‧‧Support

Claims (8)

一種電子元件密封用樹脂薄片，其利用示差掃描熱析儀測定的發熱起始溫度為120℃以上，且發熱波峰溫度為150~200℃。 A resin sheet for sealing electronic components, which has a heat generation starting temperature of 120 ° C or more and a heat generation peak temperature of 150 to 200 ° C measured by a differential scanning calorimeter. 如請求項1之電子元件密封用樹脂薄片，其在利用前述示差掃描熱析儀測定的DSC曲線中，相對於發熱波峰面積整體，在發熱波峰溫度±30℃之溫度範圍中的面積為70%以上。 The resin sheet for electronic component sealing according to claim 1, wherein the DSC curve measured by the differential scanning calorimeter has an area in the temperature range of ±30 ° C in the heat generation peak temperature with respect to the entire heat generation peak area of 70%. the above. 如請求項1之電子元件密封用樹脂薄片，其在25℃的條件下保存4週後的最低熔融黏度為保存前之最低熔融黏度的2倍以下。 The resin sheet for electronic component sealing of claim 1 which has a minimum melt viscosity after storage for 4 weeks at 25 ° C is twice or less the lowest melt viscosity before storage. 如請求項1之電子元件密封用樹脂薄片，其中，前述電子元件密封用樹脂薄片中之填充物的含量為70~90體積%。 The resin sheet for electronic component sealing according to claim 1, wherein the content of the filler in the resin sheet for electronic component sealing is 70 to 90% by volume. 如請求項1之電子元件密封用樹脂薄片，其為將環氧樹脂、酚樹脂、熱塑性樹脂、填充物及硬化促進劑捏合而獲得捏合物，並對該捏合物塑性加工成薄片狀所得者。 The resin sheet for electronic component sealing according to claim 1, which is obtained by kneading an epoxy resin, a phenol resin, a thermoplastic resin, a filler, and a curing accelerator to obtain a kneaded product, and plastically processing the kneaded product into a sheet shape. 如請求項5之電子元件密封用樹脂薄片，其中，前述硬化促進劑為咪唑系硬化促進劑。 The resin sheet for electronic component sealing according to claim 5, wherein the curing accelerator is an imidazole-based hardening accelerator. 如請求項6之電子元件密封用樹脂薄片，其中，前述咪唑系硬化促進劑為潛伏性硬化促進劑。 The resin sheet for electronic component sealing according to claim 6, wherein the imidazole-based hardening accelerator is a latent curing accelerator. 一種電子元件封裝體的製造方法，其包含下述步驟：積層步驟，係以覆蓋1個或複數個電子元件的方式將如請 求項1至7中任一項之電子元件密封用樹脂薄片積層在前述電子元件上；及密封體形成步驟，係使前述電子元件密封用樹脂薄片硬化來形成密封體。 A method of manufacturing an electronic component package, comprising the steps of: laminating a step of covering one or a plurality of electronic components The resin sheet for electronic component sealing according to any one of Items 1 to 7 is laminated on the electronic component, and the sealing body is formed by curing the resin sheet for sealing an electronic component to form a sealed body.
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