JP7452287B2 - Method for manufacturing a resin composition for sealing, resin composition for sealing, method for manufacturing an electronic component device, and electronic component device - Google Patents

Description

The present invention relates to a method for manufacturing a resin composition for sealing, a resin composition for sealing, a method for manufacturing an electronic component device, and an electronic component device.

Conventionally, in the field of element encapsulation of electronic component devices such as transistors and ICs, resin encapsulation has been mainstream from the viewpoint of productivity and cost, and resin compositions containing epoxy resins have been widely used (for example, patent documents 1). This is because the epoxy resin has an excellent balance of various properties such as workability, moldability, electrical properties, moisture resistance, heat resistance, mechanical properties, and adhesion to insert products. Furthermore, resin compositions containing epoxy resins are widely used as encapsulants in bare chip mounted electronic component devices such as COB (Chip on Board), COG (Chip on Glass), and TCP (Tape Carrier Package). .

JP 2017-115083 Publication

A sealing resin composition containing an epoxy resin, a curing agent, and an inorganic filler is produced, for example, by kneading the components constituting the sealing resin composition.
On the other hand, from the viewpoint of obtaining performance as a sealing resin composition, a sealing resin composition in which each component constituting the sealing resin composition is uniformly dispersed is desired. From the viewpoint of obtaining a sealing resin composition in which each component is uniformly dispersed, uniform kneading performance (that is, each component is uniformly dispersed by kneading) is required during the above-mentioned kneading.

One form of the present disclosure provides a method for producing a sealing resin composition that provides a sealing resin composition with high uniform dispersibility, a sealing resin composition with high uniform dispersibility, and the above-mentioned sealing resin composition. An object of the present invention is to provide a method for manufacturing an electronic component device using a sealing resin composition obtained by the manufacturing method, and an electronic component device including an element sealed with the sealing resin composition. .

Specific means for solving the above problems include the following embodiments.
<1>
preparing a dispersion containing an epoxy resin, a curing agent, an inorganic filler, a solvent, and an acetylene glycol compound;
a step of kneading the dispersion;
removing the solvent contained in the dispersion;
A method for producing a sealing resin composition having the following.
<2>
The method for producing a sealing resin composition according to <1>, wherein the acetylene glycol compound has an HLB value of 10 or less.
<3>
A sealing resin composition containing an epoxy resin, a curing agent, an inorganic filler, and an acetylene glycol compound.
<4>
The sealing resin composition according to <3>, wherein the acetylene glycol compound has an HLB value of 10 or less.
<5>
A method for manufacturing an electronic component device, comprising the step of sealing an element with a sealing resin composition produced by the method for producing a sealing resin composition according to <1> or <2>.
<6>
Motoko and
A cured product of the sealing resin composition according to <3> or <4> that seals the element;
An electronic component device comprising:

According to one aspect of the present disclosure, there is provided a method for producing a sealing resin composition that provides a sealing resin composition with high uniform dispersibility, a sealing resin composition with high uniform dispersibility, and the sealing resin. It is possible to provide a method for producing an electronic component device using a sealing resin composition obtained by the method for producing a composition, and an electronic component device including an element sealed with the sealing resin composition. .

EMBODIMENT OF THE INVENTION Hereinafter, the form for implementing this invention is demonstrated in detail. However, the present invention is not limited to the following embodiments. In the following embodiments, the constituent elements (including elemental steps and the like) are not essential unless otherwise specified. The same applies to numerical values and their ranges, and they do not limit the present invention.
In this disclosure, the term "step" includes not only a step that is independent from other steps, but also a step that cannot be clearly distinguished from other steps, as long as the purpose of the step is achieved. .
In the present disclosure, numerical ranges indicated using "~" include the numerical values written before and after "~" as minimum and maximum values, respectively.
In the numerical ranges described step by step in this disclosure, the upper limit or lower limit described in one numerical range may be replaced with the upper limit or lower limit of another numerical range described step by step. . Furthermore, in the numerical ranges described in this disclosure, the upper limit or lower limit of the numerical range may be replaced with the values shown in the Examples.
In the present disclosure, each component may contain multiple types of corresponding substances. If there are multiple types of substances corresponding to each component in the composition, the content rate or content of each component is the total content rate or content of the multiple types of substances present in the composition, unless otherwise specified. means quantity.
In the present disclosure, each component may include a plurality of types of particles. When a plurality of types of particles corresponding to each component are present in the composition, the particle diameter of each component means a value for a mixture of the plurality of types of particles present in the composition, unless otherwise specified.

[Method for producing sealing resin composition]
The method for producing a sealing resin composition of the present disclosure includes a step of preparing a dispersion containing an epoxy resin, a curing agent, an inorganic filler, a solvent, and an acetylene glycol compound (hereinafter also referred to as "dispersion preparation step"). The method includes a step of kneading the dispersion (hereinafter also referred to as "kneading step"), and a step of removing the solvent contained in the dispersion (hereinafter also referred to as "solvent removal step").

By using the method for producing a sealing resin composition of the present disclosure, a sealing resin composition with high uniform dispersibility can be obtained. Although the reason is not certain, it is assumed as follows.
The production of a sealing resin composition containing an epoxy resin, a curing agent, and an inorganic filler is carried out, for example, by kneading components that constitute the sealing resin composition (hereinafter also referred to as "constituent components"). . For example, when the constituent components include a solid component, the above-mentioned kneading is generally performed by solid-phase kneading in which the mixture is stirred while being heated to a temperature at which the solid component melts.

On the other hand, as a kneading method capable of obtaining a composition with higher uniformity of dispersion, a method of kneading a dispersion in which constituent components are dispersed in a solvent (hereinafter also referred to as "dispersion kneading method") can be considered.
In the dispersion kneading method described above, by incorporating an acetylene glycol compound into a dispersion in which the constituent components are dispersed in a solvent, a sealing resin composition with further improved uniform dispersibility can be obtained. The reason for this is presumed to be that bubbles generated during kneading of a dispersion containing a solvent are broken by the acetylene glycol compound. Specifically, if kneading is continued in a state where air bubbles are generated in the dispersion liquid, uniform kneading performance will be reduced due to the presence of air bubbles. On the other hand, when the dispersion liquid contains an acetylene glycol compound, the segment with high electron density in the molecule of the acetylene glycol compound contributes to the foam-breaking effect, and the glycol segment contributes to reducing the interfacial energy. It is thought that this suppresses the deterioration of uniform kneading properties due to air bubbles, and improves the uniform dispersibility of the resulting sealing resin composition compared to the case where no acetylene glycol compound is used.
It should be noted that a sealing resin composition with high uniform dispersibility is less likely to produce void defects during curing, and therefore tends to have a high hardness when heated and a cured product with a low coefficient of thermal expansion. A sealing resin composition with high uniform dispersibility can easily provide mechanical properties such as strength, elongation, and elasticity, dimensional stability, electrical properties, and quality stability thereof.

As described above, the method for producing a sealing resin composition of the present disclosure includes at least a dispersion preparation step, a kneading step, and a solvent removal step, and if necessary, other steps (such as those obtained after the solvent removal step) (a step of pulverizing the solid content obtained after the solvent removal step, a step of forming the solid content obtained after the solvent removal step or the pulverized product obtained by the pulverization step into a solid molded body such as a tablet shape or a sheet shape, etc.) good.
Further, the steps included in the method for manufacturing the encapsulating resin composition may be performed separately or simultaneously. Examples of embodiments in which a plurality of steps are performed simultaneously include an embodiment in which kneading is performed while removing the solvent in the kneading step and the solvent removal step.
Hereinafter, each process included in the method for producing a sealing resin composition of the present disclosure will be described in detail.

<Dispersion liquid preparation process>
In the dispersion preparation step, a dispersion containing an epoxy resin, a curing agent, an inorganic filler, a solvent, and an acetylene glycol compound is prepared.
The dispersion liquid contains an epoxy resin, a curing agent, an inorganic filler, a solvent, and an acetylene glycol compound, and if necessary, other components (a surfactant other than the acetylene glycol compound, a surfactant included in the sealing resin composition) are added. Other additives, etc.) may also be included.
Each component contained in the dispersion will be explained below.

(Epoxy resin)
The type of epoxy resin is not particularly limited as long as it has two or more epoxy groups in one molecule.
Specifically, at least one phenol selected from the group consisting of phenol compounds such as phenol, cresol, xylenol, resorcinol, catechol, bisphenol A, and bisphenol F, and naphthol compounds such as α-naphthol, β-naphthol, and dihydroxynaphthalene. Novolak type epoxy resin (phenol novolak type epoxy resin) is a product obtained by epoxidizing a novolak resin obtained by condensing or co-condensing a chemical compound with an aliphatic aldehyde compound such as formaldehyde, acetaldehyde, or propionaldehyde under an acidic catalyst. , orthocresol novolak type epoxy resin, etc.); epoxidation of triphenylmethane type phenol resin obtained by condensing or co-condensing the above phenolic compound with an aromatic aldehyde compound such as benzaldehyde or salicylaldehyde under an acidic catalyst. triphenylmethane type epoxy resin; copolymerized epoxy resin, which is obtained by epoxidizing a novolac resin obtained by cocondensing the above phenol compound and naphthol compound with an aldehyde compound under an acidic catalyst; bisphenol; A, diphenylmethane type epoxy resin which is diglycidyl ether such as bisphenol F; biphenyl type epoxy resin which is diglycidyl ether of alkyl-substituted or unsubstituted biphenol; stilbene type epoxy resin which is diglycidyl ether of stilbene type phenol compound; bisphenol Sulfur atom-containing epoxy resins that are diglycidyl ethers such as S; epoxy resins that are glycidyl ethers of alcohols such as butanediol, polyethylene glycol, and polypropylene glycol; polyhydric carboxylic acids such as phthalic acid, isophthalic acid, and tetrahydrophthalic acid. Glycidyl ester type epoxy resin, which is the glycidyl ester of a compound; Glycidylamine type epoxy resin, which has the active hydrogen bonded to the nitrogen atom of aniline, diaminodiphenylmethane, isocyanuric acid, etc. replaced with a glycidyl group; Dicyclopentadiene and phenol compound dicyclopentadiene type epoxy resin, which is the epoxidized co-condensation resin of alicyclic epoxy resins such as 2-(3,4-epoxy)cyclohexyl-5,5-spiro(3,4-epoxy)cyclohexane-m-dioxane; paraxylylene-modified epoxy which is the glycidyl ether of paraxylylene-modified phenol resin; Resin: metaxylylene-modified epoxy resin, which is the glycidyl ether of metaxylylene-modified phenolic resin; terpene-modified epoxy resin, which is the glycidyl ether of terpene-modified phenolic resin; dicyclopentadiene-modified epoxy resin, which is the glycidyl ether of dicyclopentadiene-modified phenolic resin; cyclopentadiene Cyclopentadiene-modified epoxy resin, which is the glycidyl ether of modified phenolic resin; Polycyclic aromatic ring-modified epoxy resin, which is the glycidyl ether of polycyclic aromatic ring-modified phenol resin; Naphthalene-type epoxy resin, which is the glycidyl ether of naphthalene ring-containing phenolic resin; Halogen Hydroquinone type epoxy resin; Trimethylolpropane type epoxy resin; Linear aliphatic epoxy resin obtained by oxidizing olefin bonds with peracid such as peracetic acid; Phenol aralkyl resin, naphthol aralkyl resin, etc. Aralkyl-type epoxy resins, which are obtained by epoxidizing aralkyl-type phenol resins, are included. Further examples of epoxy resins include epoxidized silicone resins and epoxidized acrylic resins. These epoxy resins may be used alone or in combination of two or more.

Among the above epoxy resins, from the viewpoint of the balance between reflow resistance and fluidity, biphenyl type epoxy resin, stilbene type epoxy resin, diphenylmethane type epoxy resin, sulfur atom-containing type epoxy resin, novolak type epoxy resin, dicyclopentadiene type epoxy resin Epoxy resins selected from the group consisting of resins, triphenylmethane type epoxy resins, copolymerized epoxy resins, and aralkyl type epoxy resins (these are referred to as "specific epoxy resins") are preferred. The specific epoxy resins may be used alone or in combination of two or more.

When the epoxy resin contains a specific epoxy resin, from the viewpoint of exhibiting the performance of the specific epoxy resin, the total content is preferably 30% by mass or more of the entire epoxy resin, and more preferably 50% by mass or more. preferable.

Among the specific epoxy resins, from the viewpoint of fluidity, biphenyl-type epoxy resins, stilbene-type epoxy resins, diphenylmethane-type epoxy resins, and sulfur atom-containing epoxy resins are more preferable, and from the viewpoint of heat resistance, dicyclopentadiene-type epoxy resins are more preferable. Epoxy resins, triphenylmethane type epoxy resins, and aralkyl type epoxy resins are preferred.

Among these, from the viewpoint of the balance of the above properties, it is preferable that the epoxy resin contains at least one selected from the group consisting of diphenylmethane type epoxy resin, biphenyl type epoxy resin, and triphenylmethane type epoxy resin; It is more preferable to use two or more of them in combination.

When the epoxy resin includes a diphenylmethane type epoxy resin, the content of the diphenylmethane type epoxy resin may be 40% by mass or more, 50% by mass or more, and 60% by mass or more based on the total mass of the epoxy resin. It may be more than % by mass. Further, the content of the diphenylmethane type epoxy resin may be 90% by mass or less, 80% by mass or less, or 70% by mass or less based on the total mass of the epoxy resin.

When the epoxy resin contains a biphenyl-type epoxy resin, the content of the biphenyl-type epoxy resin may be 10% by mass or more, 20% by mass or more, and 30% by mass or more based on the total mass of the epoxy resin. It may be more than % by mass. Further, the content of the biphenyl-type epoxy resin may be 70% by mass or less, 60% by mass or less, or 50% by mass or less based on the total mass of the epoxy resin. Further, the content of the biphenyl-type epoxy resin is preferably 30% by mass to 100% by mass, more preferably 30% by mass to 90% by mass, and 30% by mass, based on the total mass of the epoxy resin. More preferably, it is 80% by mass.

When the epoxy resin contains a triphenylmethane type epoxy resin, the content of the triphenylmethane type epoxy resin may be 30% by mass or more, and may be 40% by mass or more with respect to the total mass of the epoxy resin. The content may be 50% by mass or more. Further, the content of the triphenylmethane type epoxy resin may be 70% by mass or less, 60% by mass or less, or 50% by mass or less based on the total mass of the epoxy resin. good.

In one embodiment, the epoxy resin preferably includes a diphenylmethane type epoxy resin and a biphenyl type epoxy resin. When the epoxy resin contains a diphenylmethane type epoxy resin and a biphenyl type epoxy resin, the ratio of the diphenylmethane type epoxy resin and the biphenyl type epoxy resin is preferably 40:60 to 90:10, and 50:50 on a mass basis. The ratio is more preferably 80:20 and even more preferably 60:40 to 70:30.

In a further embodiment, the epoxy resin preferably includes a combination of a biphenyl-type epoxy resin and a triphenylmethane-type epoxy resin. When the epoxy resin includes a combination of a biphenyl-type epoxy resin and a triphenylmethane-type epoxy resin, the ratio of the biphenyl-type epoxy resin and the triphenylmethane-type epoxy resin is preferably 20:80 to 80:20 on a mass basis. The ratio is preferably 30:70 to 70:30, even more preferably 40:60 to 60:40.

Specific examples of preferred epoxy resins are shown below.

The biphenyl-type epoxy resin is not particularly limited as long as it has a biphenyl skeleton. As the biphenyl type epoxy resin, for example, an epoxy resin represented by the following general formula (II) is preferable. Among the epoxy resins represented by the following general formula (II), the 3, 3', 5, and 5' positions are methyl groups when the positions where oxygen atoms are substituted in ^R8 are the 4 and 4' positions. YX-4000H (Mitsubishi Chemical Corporation, trade name) in which all other R ^8s are hydrogen atoms, 4,4'-bis(2,3-epoxypropoxy)biphenyl, in which all R ^8s are hydrogen atoms, When all R ⁸ are hydrogen atoms, and when the 4 and 4' positions of R ⁸ are substituted with oxygen atoms, the 3, 3', 5, and 5' positions are methyl groups and the other R YL-6121H (trade name, manufactured by Mitsubishi Chemical Corporation), which is a mixture in which ⁸ is a hydrogen atom, is available as a commercial product.

In formula (II), R ⁸ represents a hydrogen atom, an alkyl group having 1 to 12 carbon atoms, or an aromatic group having 4 to 18 carbon atoms, and each of them may be the same or different. n is an average value and represents a number from 0 to 10.

The stilbene type epoxy resin is not particularly limited as long as it has a stilbene skeleton. For example, an epoxy resin represented by the following general formula (III) is preferable. Among the epoxy resins represented by the following general formula (III), the 3, 3', 5, and 5' positions are methyl groups when the positions where oxygen atoms are substituted in R ⁹ are the 4 and 4' positions. and the other R ⁹ is a hydrogen atom and all R ¹⁰ are hydrogen atoms, and three of the 3, 3', 5, and 5' positions of R ⁹ are methyl groups, ESLV-210 (Sumitomo Chemical Co., Ltd., trade name), etc., which is a mixture product in which one is a t-butyl group, the other R ⁹ is a hydrogen atom, and all R ¹⁰ are hydrogen atoms, etc. It is available as a commercial product.

In formula (III), R ⁹ and R ¹⁰ represent a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. n is an average value and represents a number from 0 to 10.

The diphenylmethane type epoxy resin is not particularly limited as long as it has a diphenylmethane skeleton. As the diphenylmethane type epoxy resin, for example, an epoxy resin represented by the following general formula (IV) is preferable. Among the epoxy resins represented by the following general formula (IV), all of R ¹¹ are hydrogen atoms, and when the positions where oxygen atoms are substituted in R ¹² are the 4 and 4' positions, 3,3 YSLV-80XY (trade name, Nippon Steel Chemical & Materials Co., Ltd.), in which the ', 5, and 5' positions are methyl groups and the other R ¹² is a hydrogen atom, is available as a commercial product.

In formula (IV), R ¹¹ and R ¹² represent a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. n is an average value and represents a number from 0 to 10.

The sulfur atom-containing epoxy resin is not particularly limited as long as it contains a sulfur atom. Examples of the sulfur atom-containing epoxy resin include epoxy resins represented by the following general formula (V). Among the epoxy resins represented by the following general formula (V), when the positions where oxygen atoms are substituted in R ¹³ are the 4 and 4' positions, the 3 and 3' positions are t-butyl groups, YSLV-120TE (trade name, Nippon Steel Chemical & Materials Co., Ltd.), in which the 6,6' positions are methyl groups and the other R ^13s are hydrogen atoms, is available as a commercial product.

In formula (V), R ¹³ represents a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and all of them may be the same or different. n is an average value and represents a number from 0 to 10.

The novolac type epoxy resin is not particularly limited as long as it is an epoxy resin obtained by epoxidizing a novolac type phenol resin. The novolak type epoxy resin is preferably an epoxy resin obtained by epoxidizing a novolak type phenol resin such as a phenol novolac resin, a cresol novolac resin, or a naphthol novolac resin using a method such as glycidyl etherification, and is represented by the following general formula (VI ) is more preferable. Among the epoxy resins represented by the following general formula (VI), all of R ¹⁴ are hydrogen atoms, R ¹⁵ is a methyl group, and i=1, ESCN-190 and ESCN-195 (Sumitomo Chemical Co., Ltd.). N-770, N-775 (DIC Corporation, product name), all of R ¹⁴ are hydrogen atoms, ⁱ = 0, YDAN-1000-10C ( _Nippon Steel Chemical & Materials Co., ^Ltd. , product a part in which all of R ¹⁴ are hydrogen atoms, i = 1, and R ¹⁵ is a methyl group, and a part in which i = 2, one of R ¹⁵ is a methyl group and one is a benzyl group HP-5600 (trade name, manufactured by DIC Corporation), which is a benzyl group-modified cresol novolac type epoxy resin having the following, is available as a commercial product.

In formula (VI), R ¹⁴ represents a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. R ¹⁵ represents a monovalent organic group having 1 to 18 carbon atoms, and all of them may be the same or different. i each independently represents an integer of 0 to 3. n is an average value and represents a number from 0 to 10.

The dicyclopentadiene type epoxy resin is not particularly limited as long as it is an epoxy resin obtained by epoxidizing a compound having a dicyclopentadiene skeleton as a raw material. For example, an epoxy resin represented by the following general formula (VII) is preferable. Among the epoxy resins represented by the following general formula (VII), HP-7200 (trade name, manufactured by DIC Corporation) in which i=0 is available as a commercial product.

In formula (VII), R ¹⁶ represents a monovalent organic group having 1 to 18 carbon atoms, and all of them may be the same or different. i each independently represents an integer of 0 to 3. n is an average value and represents a number from 0 to 10.

The triphenylmethane type epoxy resin is not particularly limited as long as it is an epoxy resin made from a compound having a triphenylmethane skeleton. The triphenylmethane type epoxy resin is preferably an epoxy resin obtained by glycidyl etherification of a triphenylmethane type phenol resin such as a novolak type phenol resin with a compound having a triphenylmethane skeleton and a compound having a phenolic hydroxyl group, and the following: Epoxy resins represented by general formula (VIII) are more preferred. Among the epoxy resins represented by the following general formula (VIII), 1032H60 (Mitsubishi Chemical Corporation, trade name) and EPPN-502H (Nippon Kayaku Co., Ltd., trade name) in which i is 0 and k is 0 etc. are available as commercial products.

In formula (VIII), R ¹⁷ and R ¹⁸ represent monovalent organic groups having 1 to 18 carbon atoms, and each may be the same or different. i each independently represents an integer of 0 to 3, and k each independently represents an integer of 0 to 4. n is an average value and represents a number from 0 to 10.

A copolymerized epoxy resin obtained by epoxidizing a novolak resin obtained from a naphthol compound, a phenol compound, and an aldehyde compound is particularly limited if it is an epoxy resin made from a compound having a naphthol skeleton or a compound having a phenol skeleton. Not done. The copolymerized epoxy resin is preferably an epoxy resin obtained by glycidyl etherification of a novolak phenol resin using a compound having a naphthol skeleton and a compound having a phenol skeleton, and an epoxy resin represented by the following general formula (IX). is more preferable. Among the epoxy resins represented by the following general formula (IX), NC-7300 (Nippon Kayaku Co., Ltd., trade name) in which R ²¹ is a methyl group, i is 1, j is 0, and k is 0 ) etc. are available as commercial products.

In formula (IX), R ¹⁹ to R ²¹ represent monovalent organic groups having 1 to 18 carbon atoms, and each of them may be the same or different. i represents an integer of 0 to 3, j represents an integer of 0 to 2, and k represents an integer of 0 to 4. l and m are each an average value and a number from 1 to 10, and (l+m) represents a number from 2 to 10. The terminal of the epoxy resin represented by formula (IX) is the following formula (IX-1) or (IX-2). In formulas (IX-1) and (IX-2), the definitions of R ¹⁹ to R ²¹ , i, j, and k are the same as the definitions of R ¹⁹ to R ²¹ , i, j, and k in formula (IX). . n is 1 (when bonding occurs via a methylene group) or 0 (when bonding does not occur via a methylene group).

The epoxy resin represented by the above general formula (IX) includes a random copolymer randomly containing l structural units and m structural units, an alternating copolymer containing alternating units, and a copolymer containing regularly , a block copolymer contained in block form, and the like. Any one of these may be used alone or two or more may be used in combination.

The copolymerizable epoxy resin is a methoxynaphthalene/cresol formaldehyde co-condensed epoxy resin containing two types of structural units in the following general formula (IX-3) in a random, alternating or block order. Epiclon HP-5000 (trade name, manufactured by DIC Corporation) represented by (IX-3) is also preferred. In the following general formula (IX-3), n and m are each an average value and a number from 1 to 10, and (n+m) is a number from 2 to 10, preferably n and m are each an average value. Yes, it is a number from 1 to 9, and (n+m) represents a number from 2 to 10.

The aralkyl type epoxy resin is composed of at least one selected from the group consisting of phenol compounds such as phenol and cresol, and naphthol compounds such as naphthol and dimethylnaphthol, and dimethoxyparaxylene, bis(methoxymethyl)biphenyl, or derivatives thereof. There are no particular limitations on the epoxy resin as long as it is an epoxy resin made from a synthesized phenol resin. The aralkyl type epoxy resin includes at least one selected from the group consisting of phenol compounds such as phenol and cresol, and naphthol compounds such as naphthol and dimethylnaphthol, and dimethoxyparaxylene, bis(methoxymethyl)biphenyl, or derivatives thereof. An epoxy resin obtained by glycidyl etherification of a phenol resin synthesized from is preferable, and an epoxy resin represented by the following general formulas (X) and (XI) is more preferable.

Among the epoxy resins represented by the following general formula (X), NC-3000S (Nippon Kayaku Co., Ltd., trade name) in which i is 0 and R ³⁸ is ^a hydrogen atom; CER-3000 (Nippon Kayaku Co., Ltd., trade name), which is a mixture of an epoxy resin in which R ⁸ is a hydrogen atom and an epoxy resin in which all R 8 in the general formula (II) are hydrogen atoms, at a mass ratio of 80:20, etc. It is available as a commercial product. Also, among the epoxy resins represented by the following general formula (XI), ESN-175 (trade name, Nippon Steel Chemical & Materials Co., Ltd.), where i is 0, j is 0, and k is 0, etc. is available as a commercial product.

In formulas (X) and (XI), R ³⁸ represents a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. R ³⁷ and R ³⁹ to R ⁴¹ each represent a monovalent organic group having 1 to 18 carbon atoms, and each of them may be the same or different. i is each independently an integer from 0 to 3; j is each independently an integer from 0 to 2; k is each independently an integer from 0 to 4; l is each independently an integer from 0 to 6. show. n is an average value, each independently a number from 0 to 10.

Regarding R ⁸ to R ²¹ and R ³⁷ to R ⁴¹ in the above general formulas (II) to (XI), "all of them may be the same or different" means, for example, 8 to R 41 in formula (II) This means that all 88 ^R8 's may be the same or different. This means that the numbers of the other R ⁹ to R ²¹ and R ³⁷ to R ⁴¹ included in the formula may be the same or different. Furthermore, R ⁸ to R ²¹ and R ³⁷ to R ⁴¹ may be the same or different. For example, all of R ⁹ and R ¹⁰ may be the same or different.
Furthermore, the monovalent organic group having 1 to 18 carbon atoms in general formulas (III) to (XI) is preferably an alkyl group or an aryl group.

In the above general formulas (II) to (XI), n is an average value, and each independently preferably ranges from 0 to 10. If n is 10 or less, the melt viscosity of the resin component will not become too high, and the viscosity of the encapsulating resin composition during melt molding will decrease, resulting in poor filling and bonding wires (gold wires that connect elements and leads). The occurrence of deformation etc. tends to be suppressed. More preferably, n is set in a range of 0 to 4.

The epoxy equivalent of the epoxy resin is not particularly limited. From the viewpoint of the balance of various properties such as moldability, reflow resistance, and electrical reliability, the epoxy equivalent of the epoxy resin is preferably 100 g/eq to 1000 g/eq, and 150 g/eq to 500 g/eq. is more preferable. The epoxy equivalent of the epoxy resin is a value measured by a method according to JIS K 7236:2009.

When the epoxy resin is solid, its softening point or melting point is not particularly limited. From the viewpoint of moldability and reflow resistance, the softening point or melting point of the epoxy resin is preferably 40°C to 180°C. More preferably, the point or melting point is 50°C to 130°C. The melting point of the epoxy resin is a value measured by differential scanning calorimetry (DSC), and the softening point of the epoxy resin is a value measured by a method (ring and ball method) according to JIS K 7234:1986.

The content of the epoxy resin (in other words, the content of the epoxy resin in the solid content of the sealing resin composition) with respect to the entire solid content (all components excluding volatile components such as solvents) of the dispersion is determined by strength, fluidity, From the viewpoint of heat resistance, moldability, etc., the content is preferably 0.5% by mass to 50% by mass, more preferably 2% by mass to 30% by mass.

(hardening agent)
Examples of the curing agent include curing agents having a phenolic hydroxyl group in the molecule (ie, phenol curing agents).
Examples of the phenol curing agent include phenol resins and polyhydric phenol compounds having two or more phenolic hydroxyl groups in one molecule.
Specific examples of phenol curing agents include polyhydric phenol compounds such as resorcinol, catechol, bisphenol A, bisphenol F, and substituted or unsubstituted biphenols; phenol, m-cresol, p-cresol, xylenol, resorcinol, catechol, and bisphenol A. , at least one phenolic compound selected from the group consisting of phenolic compounds such as bisphenol F, phenylphenol, and aminophenol, and naphthol compounds such as α-naphthol, β-naphthol, and dihydroxynaphthalene, and formaldehyde, acetaldehyde, propionaldehyde, and benzaldehyde. , and an aldehyde compound such as salicylaldehyde under an acidic catalyst; a novolac type phenolic resin obtained by condensing or co-condensing the above phenolic compound and dimethoxyparaxylene, bis(methoxymethyl)biphenyl, etc. Aralkyl type phenolic resins such as phenol aralkyl resins and naphthol aralkyl resins; paraxylylene and/or metaxylylene modified phenolic resins; melamine modified phenolic resins; terpene modified phenolic resins; Synthesized by copolymerization from the above phenolic compounds and dicyclopentadiene. dicyclopentadiene-type phenolic resin and dicyclopentadiene-type naphthol resin; cyclopentadiene-modified phenolic resin; polycyclic aromatic ring-modified phenolic resin; biphenyl-type phenolic resin; the above phenolic compounds and aromatic aldehyde compounds such as benzaldehyde and salicylaldehyde. and a triphenylmethane type phenol resin obtained by condensing or co-condensing these under an acidic catalyst; and a phenol resin obtained by copolymerizing two or more of these.
These phenol curing agents may be used alone or in combination of two or more.

Among the above phenol curing agents, from the viewpoint of reflow resistance, aralkyl type phenol resin, dicyclopentadiene type phenol resin, triphenylmethane type phenol resin, copolymerized type phenol resin of benzaldehyde type phenol resin and aralkyl type phenol resin, and at least one selected from the group consisting of novolac type phenolic resins (these are referred to as "specific phenol curing agents"). The specific phenol curing agent may be used alone or in combination of two or more.

Examples of the aralkyl type phenol resin include phenol aralkyl resins and naphthol aralkyl resins synthesized from a phenolic compound and dimethoxyparaxylene, bis(methoxymethyl)biphenyl, and the like. The aralkyl type phenol resin may be further copolymerized with other phenol resins. Copolymerized aralkyl type phenolic resins include copolymerized phenolic resins of benzaldehyde type phenol resin and aralkyl type phenol resin, copolymerized phenol resins of salicylaldehyde type phenol resin and aralkyl type phenol resin, and novolac type phenol resins. Examples include copolymerizable phenolic resins with aralkyl phenolic resins.

The aralkyl-type phenolic resin is not particularly limited as long as it is synthesized from at least one selected from the group consisting of phenolic compounds and naphthol compounds, and dimethoxyparaxylene, bis(methoxymethyl)biphenyl, or derivatives thereof. . As the aralkyl type phenol resin, phenol resins represented by the following general formulas (XII) to (XIV) are preferable.

In formulas (XII) to (XIV), R ²³ represents a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. R ²² , R ²⁴ , R ²⁵ and R ²⁸ represent a monovalent organic group having 1 to 18 carbon atoms, and each of them may be the same or different. R ²⁶ and R ²⁷ represent a hydroxyl group or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. i is each independently an integer from 0 to 3; j is each independently an integer from 0 to 2; k is each independently an integer from 0 to 4; p is each independently an integer from 0 to 4. be. n is an average value, each independently a number from 0 to 10.

Among the phenolic resins represented by the above general formula (XII), MEH-7851 (trade name, Meiwa Kasei Co., Ltd.), in which i is 0 and all R ²³ are hydrogen atoms, is available as a commercial product. .

Among the phenolic resins represented by the above general formula (XIII), i is 0 and k is 0, such as XL-225, (trade name) etc. are available as commercial products.

Among the phenolic resins represented by the above general formula (XIV), SN-170 (Nippon Steel Chemical & Materials Co., Ltd., trade name) in which j is 0, k is 0, and p is 0; 0, k is 1, ^R27 is a hydroxyl group, and p is 0, such as SN-395 (trade name, Nippon Steel Chemical & Materials Co., Ltd.), which is commercially available.

The dicyclopentadiene type phenol resin is not particularly limited as long as it is a phenol resin obtained using a compound having a dicyclopentadiene skeleton as a raw material. As the dicyclopentadiene type phenol resin, a phenol resin represented by the following general formula (XV) is preferable. Among the phenolic resins represented by the following general formula (XV), DPP (trade name, Nippon Petrochemical Co., Ltd.) in which i is 0 is available as a commercial product.

In formula (XV), R ²⁹ represents a monovalent organic group having 1 to 18 carbon atoms, and all of them may be the same or different. i each independently represents an integer of 0 to 3. n is an average value and represents a number from 0 to 10.

The triphenylmethane type phenol resin is not particularly limited as long as it is a phenol resin obtained using a compound having a triphenylmethane skeleton as a raw material. As the triphenylmethane type phenol resin, a phenol resin represented by the following general formula (XVI) is preferable.

Among the phenolic resins represented by the following general formula (XVI), MEH-7500 (trade name, Meiwa Kasei Co., Ltd.), in which i is 0 and k is 0, is available as a commercial product.

In formula (XVI), R ³⁰ and R ³¹ represent monovalent organic groups having 1 to 18 carbon atoms, and each may be the same or different. i is each independently an integer from 0 to 3, and k is each independently an integer from 0 to 4. n is an average value and is a number from 0 to 10.

The copolymerization type phenol resin of a benzaldehyde type phenol resin and an aralkyl type phenol resin is not particularly limited as long as it is a copolymerization type phenol resin of a phenol resin and an aralkyl type phenol resin obtained using a compound having a benzaldehyde skeleton as a raw material. As the copolymerization type phenol resin of a benzaldehyde type phenol resin and an aralkyl type phenol resin, a phenol resin represented by the following general formula (XVII) is preferable.

Among the phenolic resins represented by the following general formula (XVII), HE-510 (trade name, Air Water Chemical Co., Ltd.), in which i is 0, k is 0, and q is 0, is commercially available. It is available as a product.

In formula (XVII), R ³² to R ³⁴ represent monovalent organic groups having 1 to 18 carbon atoms, and each of them may be the same or different. i is each independently an integer from 0 to 3, k is each independently an integer from 0 to 4, and q is each independently an integer from 0 to 5. l and m are each an average value, and are each independently a number from 0 to 11. However, the sum of l and m is a number from 1 to 11.

The novolak type phenolic resin is particularly limited as long as it is a phenolic resin obtained by condensing or co-condensing at least one phenolic compound selected from the group consisting of phenolic compounds and naphthol compounds and an aldehyde compound under an acidic catalyst. Not done. As the novolak type phenol resin, a phenol resin represented by the following general formula (XVIII) is preferable.

Among the phenolic resins represented by the following general formula (XVIII), Tamanol 758, ⁷⁵⁹ (Arakawa Chemical Co., Ltd., trade name), HP-850N (Hitachi Chemical Co., Ltd., product name) etc. are available as commercial products.

In formula (XVIII), R ³⁵ represents a hydrogen atom or a monovalent organic group having 1 to 18 carbon atoms, and each may be the same or different. R ³⁶ represents a monovalent organic group having 1 to 18 carbon atoms, and all of them may be the same or different. i each independently represents an integer of 0 to 3. n is an average value and represents a number from 0 to 10.

For example, "all of R ²² to R ³⁶ in formulas (XII) to (XVIII) may be the same or different" means that R ²² to R 36 in formula (XII) may be the same or different from each other. This means that they can be different. This means that the numbers of the other R ²³ to R ³⁶ included in the formula may be the same or different. Further, each of R ²² to R ³⁶ may be the same or different. For example, all of R ²² and R ²³ may be the same or different, and all of R ³⁰ and R ³¹ may be the same or different.

In the above general formulas (XII) to (XVIII), n is preferably in the range of 0 to 10. If it is 10 or less, the melt viscosity of the resin component will not be too high, and the viscosity of the sealing resin composition during melt molding will be low, resulting in poor filling, deformation of bonding wires (gold wires that connect elements and leads), etc. becomes less likely to occur. The average n in one molecule is preferably set in the range of 0 to 4.

The functional group equivalent of the curing agent (in the case of a curing agent having a phenolic hydroxyl group in the molecule, the hydroxyl group equivalent) is not particularly limited. From the viewpoint of the balance of various properties such as moldability, reflow resistance, and electrical reliability, the functional group equivalent of the curing agent is preferably 70 g/eq to 1000 g/eq, and 80 g/eq to 500 g/eq. It is more preferable.
The functional group equivalent of the curing agent (in the case of a curing agent having a phenolic hydroxyl group in the molecule, the hydroxyl group equivalent) may be a value measured by a method according to JIS K 0070:1992, for example.

When the curing agent is solid, its softening point or melting point is not particularly limited. From the viewpoint of moldability and reflow resistance, the softening point or melting point of the curing agent is preferably 40°C to 180°C. More preferably, the temperature or melting point is 50°C to 130°C. In addition, the softening point or melting point of the curing agent is set at 50°C to 100°C from the viewpoint of improving fluidity and reducing the high-temperature elastic modulus of the cured product of the encapsulating resin composition to improve reflow resistance. The temperature is preferably from 50°C to 75°C, even more preferably from 50°C to 65°C.
The melting point or softening point of the curing agent is a value measured in the same manner as the melting point or softening point of the epoxy resin.

The equivalent ratio of the epoxy resin and the curing agent, that is, the ratio of the number of functional groups in the curing agent to the number of epoxy groups in the epoxy resin (number of functional groups in the curing agent/number of epoxy groups in the epoxy resin) is not particularly limited. From the viewpoint of suppressing each unreacted component, the equivalent ratio between the epoxy resin and the curing agent is preferably set in the range of 0.5 to 2.0, and is set in the range of 0.6 to 1.3. It is more preferable that From the viewpoint of moldability and reflow resistance, it is more preferable to set it in the range of 0.8 to 1.2.

(Inorganic filler)
The material of the inorganic filler is not particularly limited. Specific examples of inorganic fillers include silica (fused silica, crystalline silica, etc.), glass, alumina, calcium carbonate, zirconium silicate, calcium silicate, silicon nitride, aluminum nitride, boron nitride, beryllia, zirconia, zircon, and phosphatide. Examples include inorganic materials such as stellite, steatite, spinel, mullite, titania, talc, clay, and mica. An inorganic filler having a flame retardant effect may also be used. Examples of the inorganic filler having a flame retardant effect include aluminum hydroxide, magnesium hydroxide, composite metal hydroxides such as composite hydroxide of magnesium and zinc, zinc borate, and the like. Among these, as the inorganic filler, silica is preferred from the viewpoint of reducing the coefficient of linear expansion, and alumina is preferred from the viewpoint of high thermal conductivity. The inorganic fillers may be used alone or in combination of two or more. Examples of the inorganic filler include powder, beads made of spherical powder, fibers, and the like.
The shape of the inorganic filler is not particularly limited. From the viewpoint of fluidity of the sealing resin composition, the particle shape of the inorganic filler is preferably spherical.

In one embodiment, from the viewpoint of reflow resistance, suppression of increase in viscosity, improvement of fluidity, etc., the inorganic filler preferably contains silica, and contains silica as a main component (i.e., 50% by volume or more of the inorganic filler). It is more preferable to include.

In a further embodiment, when obtaining a cured product with high thermal conductivity, the inorganic filler preferably contains alumina, and more preferably contains alumina as a main component (i.e., 50% by volume or more of the inorganic filler). Specifically, the inorganic filler is preferably a mixture of silica and alumina, for example.

The volume average particle diameter of the entire inorganic filler is not particularly limited. The volume average particle diameter of the entire inorganic filler is preferably 0.2 μm to 80 μm, more preferably 0.5 μm to 70 μm, and even more preferably 1 μm to 50 μm. When the volume average particle diameter is 0.2 μm or more, the increase in viscosity of the sealing resin composition tends to be suppressed. When the volume average particle diameter is 80 μm or less, filling properties of the sealing resin composition into narrow gaps tend to improve. From the viewpoint of fluidity of the sealing resin composition, it is preferable that the particle size of the inorganic filler is distributed over a wide range.

The maximum particle size (also referred to as cut point) of the inorganic filler is not particularly limited. From the viewpoint of filling properties of the sealing resin composition into narrow gaps, the maximum particle size of the inorganic filler is preferably 150 μm or less, more preferably 75 μm or less, and even more preferably 55 μm or less. preferable.

The content of the inorganic filler in the entire solid content of the dispersion (all components excluding volatile components such as solvents) (that is, the content of the inorganic filler in the solid content of the sealing resin composition) is not particularly limited. The content of the inorganic filler is preferably 50% by volume or more, more preferably 60% by volume or more, even more preferably 70% by volume or more, based on the total solid volume of the dispersion. It is particularly preferable that the content is 75% by volume or more. By setting the content of the inorganic filler to 50% by volume or more of the total solid content of the dispersion, properties such as thermal expansion coefficient, thermal conductivity, and elastic modulus of the cured product of the sealing resin composition are suitably improved. It tends to be possible to do so.
Further, the content of the inorganic filler is preferably 95% by volume or less, more preferably 90% by volume or less, and even more preferably 87% by volume or less based on the total solid volume of the dispersion. preferable. When the content of the inorganic filler is 95% by volume or less of the total solid content of the dispersion, the increase in viscosity of the sealing resin composition is suppressed, the fluidity is further improved, and the moldability is improved. There is a tendency.
From the above viewpoint, the content of the inorganic filler is preferably 50% to 95% by volume, more preferably 60% to 95% by volume, based on the total volume of the solid content of the dispersion. It is more preferably 70% to 95% by volume, particularly preferably 75% to 90% by volume, and most preferably 80% to 87% by volume.

Note that the average particle diameter of the inorganic filler in the present disclosure is the volume average particle diameter.
The average particle size of the inorganic filler in the present disclosure can be measured as a volume average particle size (D50) using a laser diffraction scattering particle size distribution measuring device.
Moreover, the average particle diameter of the inorganic filler in the dispersion, the sealing resin composition, or the cured product thereof can be specifically measured by the following method. A crucible containing the dispersion liquid, the sealing resin composition, or a cured product thereof is placed in a muffle furnace and heated to 800°C. Leave the sample for 4 hours until completely incinerated. The sample is naturally cooled until it returns to room temperature (25°C), and the ash (inorganic filler) is extracted. Prepare a dispersion by sufficiently dispersing the inorganic filler using an ultrasonic disperser or the like. Using this dispersion, the volume average particle diameter of the inorganic filler can be measured from the volume-based particle size distribution measured by a laser diffraction scattering particle size distribution measuring device.

In the present disclosure, "using two or more types of inorganic fillers in combination" means, for example, when two or more types of inorganic fillers with the same ingredients but different average particle sizes are used, inorganic fillers with the same average particle size and different ingredients Examples include cases in which two or more types of fillers are used, and cases in which two or more types of inorganic fillers with different average particle diameters and types are used.

(solvent)
The solvent contained in the dispersion liquid is not particularly limited, and it is preferable that the solvent has the property of uniformly dissolving or dispersing each component constituting the sealing resin composition.
Examples of the solvent include water, organic solvents, and the like. Examples of organic solvents include dimethylformamide, dimethylacetamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, diethylene glycol dimethyl ether, toluene, benzene, xylene, methyl ethyl ketone, methyl isobutyl ketone, tetrahydrofuran, ethyl cellosolve, ethyl cellosolve acetate, butyl cellosolve, dioxane, Examples include cyclohexanone and ethyl acetate. These solvents may be used alone or in combination of two or more.

The boiling point of the solvent contained in the dispersion is preferably 130°C or lower, more preferably 110°C or lower, and even more preferably 90°C or lower, from the viewpoint of ease of removing the solvent in the solvent removal step described below. Further, the boiling point of the solvent contained in the dispersion liquid is preferably 50°C or higher, more preferably 60°C or higher, and even more preferably 70°C or higher, from the viewpoint of ease of handling and uniform kneading.
That is, the boiling point of the solvent is preferably in the range of 50°C to 130°C, more preferably in the range of 60°C to 110°C, even more preferably in the range of 70°C to 90°C.

The content of the solvent in the entire dispersion is preferably 80% by mass or less, more preferably 50% by mass or less, and even more preferably 30% by mass or less, from the viewpoint of ease of removing the solvent in the solvent removal step described below. In addition, the content of the solvent in the entire dispersion is preferably 5% by mass or more, more preferably 10% by mass or more, and even more preferably 20% by mass or more from the viewpoint of uniform kneading properties.
That is, the content of the solvent in the entire dispersion is preferably in the range of 5% by mass to 80% by mass, more preferably in the range of 10% by mass to 50% by mass, and even more preferably in the range of 20% by mass to 30% by mass.

(Acetylene glycol compound)
The acetylene glycol compound is not particularly limited as long as it is acetylene glycol and its derivatives.
Examples of the acetylene glycol include unsaturated glycols having a carbon-carbon triple bond, such as a compound represented by the following general formula (A1).
Further, examples of derivatives of acetylene glycol include ethylene oxide adducts of acetylene glycol, and specifically, examples include compounds represented by the following general formula (A2).

In general formulas (A1) and (A2), R ⁵¹ to R ⁵⁸ each independently represent an alkyl group, m and n each independently represent an integer of 0 to 25, and 1≦m+n≦50.

The alkyl groups represented by R ⁵¹ to R ⁵⁸ in general formulas (A1) and (A2) are each independently preferably an alkyl group having 1 to 6 carbon atoms. Further, it is more preferable that one of R ⁵¹ and R ⁵² in general formula (A1) is an alkyl group having 1 to 3 carbon atoms and the other is an alkyl group having 3 to 6 carbon atoms, and one is methyl. More preferably, the other group is a branched alkyl group having 3 to 5 carbon atoms. Regarding R ⁵³ and R ⁵⁴ in general formula (A1), R ⁵⁵ and R ⁵⁶ in general formula (A2), and R ⁵⁷ and R ⁵⁸ in general formula (A2), R in general formula (A1) ⁵¹ and ^R52 .
From the viewpoint of adjusting the HLB value to 10 or less, m and n in the general formula (A2) preferably satisfy 1≦m+n≦10, and more preferably 1≦m+n≦4.

Specific examples of acetylene glycol compounds include 2,4,7,9-tetramethyl-5-decyne-4,7-diol, 3,6-dimethyl-4-decyne-3,6-diol, and 3,6-diol. -dimethyl-4-octyne-3,6-diol, 2,5-dimethyl-3-hexyne-2,5-diol, and ethylene oxide adducts of these acetylene glycols.
Acetylene glycol compounds may be used alone or in combination of two or more.

The HLB value (i.e., Hydrophile-Lipophile Balance) of the acetylene glycol compound is determined from the viewpoint of achieving both uniform dispersibility of the sealing resin composition and ease of removal in the solvent removal process. , preferably from 1 to 10, more preferably from 2 to 8, even more preferably from 4 to 8.

There are several methods known to calculate the HLB value, such as those described in Takehiko Fujimoto, "Completely Revised Edition New Introduction to Surfactants" (Sanyo Chemical Industries, Ltd., published October 1981). . In this specification, a value calculated by the following calculation formula (A) is used as the HLB value.
Formula (A): HLB value = (molecular weight of hydrophilic part/molecular weight of entire compound) x 100/5
In addition, the "hydrophilic moiety" in the above formula (A) means a partial structure exhibiting hydrophilicity among the acetylene glycol compounds. Specifically, for example, the hydrophilic moiety in the compound represented by general formula (A1) is a hydroxyl group (i.e., two "-OH") in the side chain, and the hydrophilic moiety in the compound represented by general formula (A2) is The functional moieties are side chain ethylene glycol chains and hydroxyl groups (ie, "-(OC ₂ H ₄ ) _m --OH" and "-(OC ₂ H ₄ ) _n --OH").

The content of the acetylene glycol compound in the entire dispersion is preferably in the range of 0.01% by mass to 1% by mass, and 0.05% by mass from the viewpoint of obtaining uniform dispersibility of the sealing resin composition. The range is more preferably from 0.5% by mass to 0.5% by mass, and even more preferably from 0.05% to 0.3% by mass.
In addition, the content of the acetylene glycol compound based on 100 parts by mass of the solvent contained in the dispersion liquid should be in the range of 0.01 parts by mass to 20 parts by mass from the viewpoint of obtaining uniform dispersibility of the sealing resin composition. It is preferably in the range of 0.1 parts by mass to 50 parts by mass, and even more preferably in the range of 0.3 parts by mass to 1.5 parts by mass.

(Other additives)
-Other surfactants-
The dispersion liquid may contain a surfactant other than the acetylene glycol compound (hereinafter also referred to as "other surfactant") as necessary, or may not contain any other surfactant.
The type of other surfactants is not particularly limited, and surfactants commonly used in organic resin compositions for electronic components can be used. Other surfactants include nonionic surfactants, anionic surfactants, fluorine-based surfactants, and the like. When using other surfactants, one type may be used alone, or two or more types may be used in combination.

Examples of nonionic surfactants include polyoxyalkylene alkyl ether surfactants such as polyoxyethylene alkyl ether, sorbitan fatty acid ester surfactants, polyoxyethylene sorbitan fatty acid ester surfactants, and polyoxyethylene sorbitol fatty acid ester surfactants. Active agent, glycerin fatty acid ester surfactant, polyoxyethylene fatty acid ester surfactant, polyoxyethylene alkylamine surfactant, alkyl alkanolamide surfactant, polyether modified silicone surfactant, aralkyl modified silicone surfactant, Examples include polyester-modified silicone surfactants, polyacrylic surfactants, and the like. Among these, preferred nonionic surfactants are polyether-modified silicone surfactants and aralkyl-modified silicone surfactants.
Examples of anionic surfactants include alkylbenzene sulfonates, alkylphenyl sulfonates, alkylnaphthalene sulfonates, higher fatty acid salts, higher fatty acid ester sulfate salts, higher fatty acid ester sulfonate salts, and higher alcohol ether salts. Examples include sulfuric ester salts and sulfonic acid salts, higher alkyl sulfosuccinates, polyoxyethylene alkyl ether carboxylates, polyoxyethylene alkyl ether sulfates, alkyl phosphates, polyoxyethylene alkyl ether phosphates, and the like.
As the fluorine-based surfactant, a compound having a fluorine atom in the hydrophobic part and a hydrophilic part such as a cationic group, anionic group, hydroxyl group, or ether bond in the hydrophilic part is preferable, such as a perfluoroalkyl group-containing carboxylic acid. , perfluoroalkyl group-containing sulfonic acid, perfluoroalkyl group-containing phosphoric acid (ester), perfluoroalkyl group-containing oxide adduct, perfluoroalkyl group-containing ammonium, and other compounds having a perfluoroalkyl group as the hydrophobic moiety. It will be done.

-Curing accelerator-
A curing accelerator may be used as another additive to be included in the encapsulating resin composition to be produced.
The type of curing accelerator is not particularly limited, and can be selected depending on the type of epoxy resin, desired characteristics of the sealing resin composition, and the like.

As curing accelerators, diazabicycloalkenes such as 1,5-diazabicyclo[4.3.0]nonene-5 (DBN) and 1,8-diazabicyclo[5.4.0]undecene-7 (DBU); Cyclic amidine compounds such as 2-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, and 2-heptadecyl imidazole; derivatives of the cyclic amidine compounds; phenol novolac salts of the cyclic amidine compounds or derivatives thereof; Compounds include maleic anhydride, 1,4-benzoquinone, 2,5-torquinone, 1,4-naphthoquinone, 2,3-dimethylbenzoquinone, 2,6-dimethylbenzoquinone, 2,3-dimethoxy-5-methyl-1 , 4-benzoquinone, 2,3-dimethoxy-1,4-benzoquinone, phenyl-1,4-benzoquinone, and other quinone compounds, and diazophenylmethane, which have intramolecular polarization by adding a compound with a π bond, such as diazophenylmethane. Compounds: Cyclic amidinium compounds such as DBU tetraphenylborate salt, DBN tetraphenylborate salt, 2-ethyl-4-methylimidazole tetraphenylborate salt, N-methylmorpholine tetraphenylborate salt; pyridine, triethylamine, Tertiary amine compounds such as ethylenediamine, benzyldimethylamine, triethanolamine, dimethylaminoethanol, tris(dimethylaminomethyl)phenol; derivatives of the above tertiary amine compounds; tetra-n-butylammonium acetate, tetra-n-phosphate Ammonium salt compounds such as butylammonium, tetraethylammonium acetate, tetra-n-hexylammonium benzoate, and tetrapropylammonium hydroxide; triphenylphosphine, diphenyl(p-tolyl)phosphine, tris(alkylphenyl)phosphine, tris(alkoxyphenyl) ) phosphine, tris(alkyl alkoxyphenyl)phosphine, tris(dialkylphenyl)phosphine, tris(trialkylphenyl)phosphine, tris(tetraalkylphenyl)phosphine, tris(dialkoxyphenyl)phosphine, tris(trialkoxyphenyl)phosphine , tris(tetraalkoxyphenyl)phosphine, trialkylphosphine, dialkylarylphosphine, alkyldiarylphosphine, and other tertiary phosphines; phosphine compounds such as complexes of the tertiary phosphine and organic borons; the tertiary phosphine or the phosphine compound and maleic anhydride, 1,4-benzoquinone, 2,5-torquinone, 1,4-naphthoquinone, 2,3-dimethylbenzoquinone, 2,6-dimethylbenzoquinone, 2,3-dimethoxy-5-methyl-1,4 - A compound having intramolecular polarization obtained by adding a compound with a π bond, such as a quinone compound such as benzoquinone, 2,3-dimethoxy-1,4-benzoquinone, or phenyl-1,4-benzoquinone, or diazophenylmethane; The tertiary phosphine or the phosphine compound and 4-bromophenol, 3-bromophenol, 2-bromophenol, 4-chlorophenol, 3-chlorophenol, 2-chlorophenol, 4-iodinated phenol, 3-iodinated phenol , 2-iodinated phenol, 4-bromo-2-methylphenol, 4-bromo-3-methylphenol, 4-bromo-2,6-dimethylphenol, 4-bromo-3,5-dimethylphenol, 4-bromo -Halogenated phenol compounds such as 2,6-di-t-butylphenol, 4-chloro-1-naphthol, 1-bromo-2-naphthol, 6-bromo-2-naphthol, 4-bromo-4'-hydroxybiphenyl Compounds with intramolecular polarization obtained through the dehydrohalogenation process after reacting; tetra-substituted phosphonium such as tetraphenylphosphonium, and no phenyl group bonded to a boron atom such as tetra-p-tolylborate. Examples include tetra-substituted phosphonium and tetra-substituted borate; salts of tetraphenylphosphonium and phenol compounds, and the like.
Among these, the curing accelerator preferably contains a phosphorus curing accelerator, and more preferably contains a phosphonium compound. One type of curing accelerator may be used alone, or two or more types may be used in combination.

When using a curing accelerator, the content of the curing accelerator is preferably 0.1 parts by mass to 30 parts by mass based on 100 parts by mass of the resin component (i.e., the total of the epoxy resin and the curing agent), and 1 More preferably, the amount is from parts by mass to 15 parts by mass. When the amount of the curing accelerator is 0.1 parts by mass or more based on 100 parts by mass of the resin component, a sealing resin composition that cures well in a short time tends to be obtained. When the amount of the curing accelerator is 30 parts by mass or less based on 100 parts by mass of the resin component, a sealing resin composition that does not have an excessively fast curing rate and can yield a good molded product tends to be obtained.

-Coupling agent-
In order to improve the adhesion between the resin component and the inorganic filler in the encapsulating resin composition to be produced, a coupling agent may be used as another additive to be contained in the encapsulating resin composition.
Examples of the coupling agent include known coupling agents such as silane compounds such as epoxysilane, mercaptosilane, aminosilane, alkylsilane, ureidosilane, and vinylsilane, titanium compounds, aluminum chelate compounds, and aluminum/zirconium compounds. .

When using a coupling agent, the amount of the coupling agent is preferably 0.05 parts by mass to 5 parts by mass, and 0.1 parts by mass to 2.5 parts by mass, based on 100 parts by mass of the inorganic filler. It is more preferable that there be. When the amount of the coupling agent is 0.05 parts by mass or more based on 100 parts by mass of the inorganic filler, a sealing resin composition that has improved adhesiveness to the frame tends to be obtained. When the amount of the coupling agent is 5 parts by mass or less with respect to 100 parts by mass of the inorganic filler, a sealing resin composition with improved package moldability tends to be obtained.

-Ion exchanger-
An ion exchanger may be used as another additive to be contained in the sealing resin composition to be produced. From the viewpoint of improving the moisture resistance and high-temperature storage characteristics of an electronic component device including an element to be sealed, it is preferable that the sealing resin composition contains an ion exchanger.
The ion exchanger is not particularly limited, and conventionally known ones can be used. Specific examples include hydrotalcite compounds, and hydrous oxides of at least one element selected from the group consisting of magnesium, aluminum, titanium, zirconium, and bismuth. One type of ion exchanger may be used alone, or two or more types may be used in combination. Among them, hydrotalcite represented by the following general formula (A) is preferred.

Mg _(1-X) Al _X (OH) ₂ (CO ₃ ) _X/2・mH ₂ O ... (A)
(0<X≦0.5, m is a positive number)

When using an ion exchanger, its content is not particularly limited as long as it is sufficient to trap ions such as halogen ions. For example, the content of the ion exchanger is preferably 0.1 parts by mass to 30 parts by mass, more preferably 1 part by mass to 15 parts by mass, based on 100 parts by mass of the resin component.

-Release agent-
From the viewpoint of obtaining good mold releasability from the mold during molding, a mold release agent may be used as another additive to be included in the encapsulating resin composition to be produced.
The mold release agent is not particularly limited, and conventionally known ones can be used. Specific examples include carnauba wax, higher fatty acids such as montanic acid and stearic acid, higher fatty acid metal salts, ester waxes such as montanic acid esters, and polyolefin waxes such as oxidized polyethylene and non-oxidized polyethylene. One type of mold release agent may be used alone, or two or more types may be used in combination.

When using a mold release agent, the amount thereof is preferably 0.01 parts by mass to 15 parts by mass, more preferably 0.1 parts by mass to 10 parts by mass, based on 100 parts by mass of the resin component. When the amount of the mold release agent is 0.01 part by mass or more based on 100 parts by mass of the resin component, a sealing resin composition that provides sufficient mold release properties tends to be obtained. When the amount of the mold release agent is 15 parts by mass or less based on 100 parts by mass of the resin component, a sealing resin composition that provides better adhesiveness tends to be obtained.

-Flame retardants-
A flame retardant may be used as another additive to be included in the encapsulating resin composition to be produced.
The flame retardant is not particularly limited, and conventionally known flame retardants can be used. Specifically, organic or inorganic compounds containing a halogen atom, an antimony atom, a nitrogen atom, or a phosphorus atom, metal hydroxides, and the like can be mentioned. One type of flame retardant may be used alone, or two or more types may be used in combination.

When a flame retardant is used, the amount thereof is not particularly limited as long as it is sufficient to obtain the desired flame retardant effect. The amount of the flame retardant is preferably 1 part by mass to 300 parts by mass, more preferably 2 parts by mass to 150 parts by mass, based on 100 parts by mass of the resin component.

-Coloring agent-
A coloring agent may be used as another additive to be included in the encapsulating resin composition to be manufactured.
Examples of the colorant include known colorants such as carbon black, organic dyes, organic pigments, titanium oxide, red lead, and red iron. The content of the colorant can be appropriately selected depending on the purpose and the like. One type of coloring agent may be used alone, or two or more types may be used in combination.

-Stress reliever-
As other additives to be included in the produced sealing resin composition, stress relaxation agents such as silicone oil and silicone rubber particles may be used. When the encapsulating resin composition contains a stress relaxation agent, it is possible to further reduce the warpage of the package and the occurrence of package cracks.
Examples of the stress relaxation agent include commonly used stress relaxation agents (flexibility agents). Specific examples of stress relaxation agents include thermoplastic elastomers such as silicone-based, styrene-based, olefin-based, urethane-based, polyester-based, polyether-based, polyamide-based, and polybutadiene-based, NR (natural rubber), and NBR (acrylonitrile-butadiene). rubber), acrylic rubber, urethane rubber, rubber particles such as silicone powder, methyl methacrylate-styrene-butadiene copolymer (MBS), methyl methacrylate-silicone copolymer, methyl methacrylate-butyl acrylate copolymer, etc. Examples include rubber particles having a core-shell structure. One type of stress relaxation agent may be used alone, or two or more types may be used in combination. Among these, silicone stress relievers are preferred. Examples of the silicone stress relaxation agent include those having an epoxy group, those having an amino group, and those modified with polyether.

(Preparation method of dispersion)
The method for preparing the dispersion liquid is not particularly limited, and examples thereof include a method of mixing the above-mentioned components contained in the dispersion liquid in predetermined amounts using a mixer or the like.
The temperature during preparation of the dispersion is not particularly limited, and may be, for example, 5°C to 50°C.
When stirring is performed during the preparation of the dispersion, the stirring time is not particularly limited, and may be, for example, 10 minutes to 120 minutes.

<Kneading process>
In the kneading step, the dispersion prepared in the dispersion preparation step is kneaded. Specifically, the dispersion is kneaded using a stirrer, a miller, a three-roll mill, a ball mill, a bead mill, a homodisper, a kneader, a roll, an extruder, or the like.
From the viewpoint of promoting kneading and suppressing thermal deterioration of the dispersion liquid components, the kneading temperature is, for example, in the range of 40°C to 140°C, preferably in the range of 60°C to 120°C, and more preferably in the range of 80°C to 110°C. .
The kneading time is, for example, in the range of 1 minute to 60 minutes, preferably in the range of 5 minutes to 30 minutes, and preferably in the range of 5 minutes to 20 minutes, from the viewpoint of balancing kneading properties and progress of thermal deterioration of the dispersion liquid components. is more preferable.
In addition, in a kneading process, you may perform the solvent removal process mentioned later.

<Solvent removal process>
In the solvent removal step, the solvent contained in the dispersion prepared in the dispersion preparation step is removed. Specifically, the solvent is evaporated and removed from the dispersion by heating the dispersion, reducing pressure, or the like.
When removing the solvent by heating, the heating temperature is, from the viewpoint of reducing residual solvent and promoting kneading, for example, in the range of 40°C to 140°C, preferably in the range of 60°C to 120°C, and in the range of 80°C to 110°C. The range is more preferred. Further, from the viewpoint of reducing residual solvent and promoting kneading, the heating time is, for example, in the range of 1 minute to 60 minutes, preferably in the range of 5 minutes to 30 minutes, and more preferably in the range of 5 minutes to 20 minutes.
When removing the solvent by reduced pressure, the degree of reduced pressure is preferably in the range of 0 MPa to 0.07 MPa, more preferably in the range of 0 MPa to 0.05 MPa, from the viewpoint of reducing residual solvent. Further, from the viewpoint of promoting kneading in addition to reducing residual solvent, the decompression time is, for example, in the range of 1 minute to 60 minutes, preferably in the range of 5 minutes to 30 minutes, and more preferably in the range of 5 minutes to 20 minutes.
In addition, in the solvent removal step, the solvent may be removed by performing both heating and depressurization. Moreover, the solvent removal step may be performed in the above-mentioned kneading step.

In the solvent removal step, it is sufficient that at least a portion of the solvent contained in the dispersion is removed. The amount of solvent removed in the solvent removal step is preferably 99% by mass or more, more preferably 99.5% by mass or more, and 99.9% by mass, based on the entire solvent contained in the dispersion. It is more preferable that it is above.

[Sealing resin composition]
The sealing resin composition of the present disclosure contains an epoxy resin, a curing agent, an inorganic filler, and an acetylene glycol compound, and may contain other additives as necessary.
Examples of the sealing resin composition of the present disclosure include the sealing resin composition produced by the method for producing a sealing resin composition described above.
The epoxy resin, curing agent, inorganic filler, and other additives contained in the encapsulating resin composition of the present disclosure are the epoxy resin, curing agent, and other additives contained in the dispersion used in the method for producing the encapsulating resin composition described above. The additives are as described above as additives, inorganic fillers, and other additives.

Furthermore, the type of acetylene glycol compound contained in the encapsulating resin composition of the present disclosure is the same as the acetylene glycol compound contained in the dispersion liquid used in the method for producing the encapsulating resin composition described above. Ru.
The content of the acetylene glycol compound contained in the encapsulating resin composition is, for example, 100 ppm or less, preferably 2 ppm to 50 ppm, and 3 ppm to 20 ppm, based on the entire encapsulating resin composition. It is more preferable that the range is within the range.

Here, the content of the acetylene glycol compound contained in the sealing resin composition is measured as follows.
The mass at 250°C of a comparison sample that is a sealing resin composition that does not contain an acetylene glycol compound, and the mass at 250°C of a measurement sample that is a sealing resin composition that contains an acetylene glycol compound. The mass when heated is measured, and the difference in mass is calculated as the mass of the acetylene glycol compound contained in the sealing resin composition. Then, the calculated mass of the acetylene glycol compound contained in the encapsulating resin composition is divided by the mass of the measurement sample at room temperature (25°C) before measurement, and the amount of the acetylene glycol compound contained in the encapsulating resin composition is calculated. The content of acetylene glycol compounds.
The comparative sample is a sealing resin composition having the same composition as the measurement sample above, except that it does not contain an acetylene glycol compound. The comparative sample can be obtained, for example, by going through the same steps as the method for producing the measurement sample, except that no acetylene glycol compound is used in the dispersion preparation step.

The measurement and calculation of the mass during heating (hereinafter referred to as "thermal weight") is performed as follows.
Specifically, thermogravimetric analysis (TG-DTA) can be used. For example, using the following equipment and conditions, thermogravimetric analysis is performed to measure the thermogravimetry of the encapsulating resin composition, and the amount of acetylene glycol compound contained in the encapsulating resin composition is determined by the following formula (1). Calculate content.
・Measurement conditions device: TG/DTA 7300 (manufactured by Seiko Instruments Inc.)
Sample amount: 0.01g
Heating atmosphere: Nitrogen 100ml/min Heating start temperature: 20℃
Heating end temperature: 300℃
Heating rate: 10℃/min

・Calculation C = ((W1-W2) / W) × 10 ⁶ ...(1)
C: Content rate (ppm) of acetylene glycol compounds contained in the measurement sample
W1: Mass (g) of comparative sample at 250°C measured by thermogravimetric analysis
W2: Mass (g) of the measurement sample at 250°C measured by thermogravimetric analysis (TG-DTA)
W: Mass of measurement sample (0.01g)

The sealing resin composition is preferably solid at room temperature and pressure (for example, 25° C. and atmospheric pressure). When the resin composition for sealing is solid, the shape is not particularly limited, and examples thereof include powder, granule, tablet, and the like. In the case where the sealing resin composition is in the form of a tablet, it is preferable from the viewpoint of handleability that the dimensions and mass are such that they match the molding conditions of the package.

The coefficient of thermal expansion (hereinafter referred to as CTE) when the sealing resin composition is made into a cured product is not particularly limited, and is preferably 6 ppm/°C or less, more preferably 5 ppm/°C or less, It is more preferably 4 ppm/°C or less, particularly preferably 3 ppm/°C or less.
CTE measurement is performed as follows. Specifically, the TMA method (differential expansion method) can be used. Specifically, a sealing resin composition was molded using a transfer molding machine and a rectangular mold under the conditions of a molding temperature of 175°C, a molding time of 90 seconds, and a pressure of 7 MPa, and was further molded at 175°C for 3 hours. Post-curing is performed under the following conditions to prepare a test piece for TMA measurement with dimensions: 4 mm (W) x 4 mm (D) x 0.2 mm (H). The dimension of the above test piece in the W direction was measured using a thermomechanical analyzer (Q400) manufactured by TA Instruments in a temperature range of 25 to 300°C using the compression method (load 0.05N) at a heating rate of 5°C. The temperature is measured at a rate of 200°C to 240°C, and the CTE is calculated in the temperature range of 200 to 240°C.

The hardness when heated when the sealing resin composition is cured is not particularly limited. The hardness when heated is preferably 60 or more, more preferably 65 or more, even more preferably 70 or more, and particularly preferably 75 or more.
Measurement of hot hardness is performed as follows. Specifically, using a transfer molding machine and a disk mold, the sealing resin composition was molded at 175°C for 90 seconds and under a pressure of 7 MPa, and then post-cured at 175°C for 3 hours. A disk-shaped test piece for hot hardness measurement with a size of 50 mm in diameter and 3 mm in thickness is prepared. The hot hardness (180° C.) of the disk-shaped test piece is measured using a Shore D hardness meter (manufactured by Kobunshi Keiki Co., Ltd.).

[Electronic component device, method for manufacturing electronic component device]
An electronic component device according to an embodiment of the present disclosure includes an element and a cured product of the above-mentioned sealing resin composition that seals the element.
Electronic component devices include lead frames, pre-wired tape carriers, wiring boards, glass, silicon wafers, organic substrates, and other supporting members, as well as elements (semiconductor chips, active elements such as transistors, diodes, and thyristors, capacitors, and resistors). , a passive element such as a coil, etc.) and the obtained element part is sealed with a sealing resin composition.
More specifically, after fixing the element on a lead frame and connecting the terminal part of the element such as a bonding pad and the lead part with wire bonding, bumps, etc., the element is transferred by transfer molding using a sealing resin composition. DIP (Dual Inline Package), PLCC (Plastic Leaded Chip Carrier), QFP (Quad Flat Package), SOP (Small Outline Package), SOJ (Small l Outline J-lead package), TSOP (Thin Small Outline TCP (Tape Carrier Package), which has a structure in which an element connected to a tape carrier with bumps is sealed with a sealing resin composition; COB (Chip On Board) modules, hybrid ICs, and multichips that have a structure in which elements are connected to wiring formed on a support member by wire bonding, flip chip bonding, soldering, etc., and sealed with a sealing resin composition. Module, etc.: After mounting an element on the surface of a support member with terminals for wiring board connection formed on the back side and connecting the element and wiring formed on the support member by bumps or wire bonding, a resin composition for sealing is applied. Examples include BGA (Ball Grid Array), CSP (Chip Size Package), MCP (Multi Chip Package), etc., which have a structure in which elements are sealed. Moreover, the sealing resin composition can also be suitably used in printed wiring boards.

A method for manufacturing an electronic component device according to an embodiment of the present disclosure includes a step of sealing an element with a sealing resin composition produced by the above-described method for producing a sealing resin composition.
Examples of methods for sealing an element using the sealing resin composition include low-pressure transfer molding, injection molding, compression molding, and the like. Among these, low pressure transfer molding is common.

EXAMPLES Hereinafter, the present invention will be specifically explained with reference to Examples, but the present invention is not limited to these Examples.

[Preparation of dispersion]
The following materials were mixed in the compositions (parts by mass) listed in Tables 1 and 2, and stirred for 60 minutes at 25° C. using an inclined paddle blade stirrer as a stirring device.
Note that a blank column in Tables 1 and 2 means that the component was not blended. Further, Tables 1 and 2 show the content (by volume) of the inorganic filler relative to the entire solid content (all components excluding volatile components such as solvents) of the dispersion.

(Epoxy resin)
Epoxy resin 1: Triphenylmethane type epoxy resin (epoxy equivalent: 167 g/eq, softening point: 59°C, Mitsubishi Chemical Corporation, product name: 1032H60, epoxy resin represented by general formula (VIII))
Epoxy resin 2: Phenol aralkyl type epoxy resin (epoxy equivalent: 275 g/eq, softening point: 58°C, Nippon Kayaku Co., Ltd., trade name: NC-3000, epoxy resin represented by general formula (X))
Epoxy resin 3: Mixture of triphenylmethane type epoxy resin and biphenyl type epoxy resin (epoxy equivalent: 237 g/eq, softening point: 93°C, Nippon Kayaku Co., Ltd., product name: CER-3000, represented by general formula (X) (Content of epoxy resin: 80% by mass)

(hardening agent)
Curing agent 1: Phenol curing agent which is a triphenylmethane type phenol resin (hydroxyl equivalent: 103 g/eq, softening point: 85°C, Meiwa Kasei Co., Ltd., trade name: MEH7500-3S, compound represented by general formula (XVI))
Curing agent 2: Phenol curing agent which is a naphthol aralkyl type phenolic resin (hydroxyl equivalent: 210 g/eq, softening point: 85°C, Nippon Steel Chemical & Materials Co., Ltd., product name: SN-485, represented by general formula (XIV) Compound)
Curing agent 3: Phenol curing agent which is a phenol aralkyl type phenol resin (hydroxyl equivalent: 174 g/eq, softening point: 75°C, Meiwa Kasei Co., Ltd., trade name: MEHC7800-S, compound represented by general formula (XIII))

(Inorganic filler)
Fused silica (spherical fused silica, average particle diameter 17.5 μm, specific surface area 3.8 m ² /g)

(solvent)
Methyl ethyl ketone (boiling point 79°C)

(Acetylene glycol compound)
Acetylene glycol compound 1: Compound name: ethylene oxide adduct of 2,4,7,9-tetramethyl-5-decyne-4,7-diol, (Air Products Co., Ltd., product name: Surfynol 420, HLB: 4. 0)
Acetylene glycol compound 2: Compound name: ethylene oxide adduct of 2,4,7,9-tetramethyl-5-decyne-4,7-diol, (Air Products Co., Ltd., product name: Surfynol 440, HLB: 8. 0)
Acetylene glycol compound 3: Compound name: ethylene oxide adduct of 2,4,7,9-tetramethyl-5-decyne-4,7-diol, (Nissin Chemical Industry Co., Ltd., product name: Olfine E1004, HLB: 8 .0)

(surfactant)
Surfactant 1: Organic fluorine compound (DIC, trade name: Megafac F-477, nonionic surfactant)

(hardening accelerator)
Curing accelerator 1: Addition reaction product of tributylphosphine and 1,4-benzoquinone Curing accelerator 2: 2-ethyl-4-methylimidazole

(coupling agent)
Coupling agent: N-phenyl-3-aminopropyltrimethoxysilane (Shin-Etsu Chemical Co., Ltd., trade name "KBM-573")
(colorant)
Carbon black (Mitsubishi Chemical Corporation, product name "MA600")
(Release agent)
Montanic acid ester wax (Clariant Japan Co., Ltd., product name “HW-E”)

[Kneading and solvent removal]
The resulting dispersion is kneaded with rolls under the conditions of a reduced pressure of 0.02 MPa, a kneading temperature of 100°C, and a kneading time of 10 minutes, thereby simultaneously kneading the dispersion and removing the solvent (removal of the solvent by heating). In this way, a sealing resin composition was obtained.

[Measurement and evaluation]
Regarding the obtained encapsulating resin composition, the content of the acetylene glycol compound in the entire encapsulating resin composition, the coefficient of thermal expansion, and the hardness when heated were measured by the methods described above. The results are shown in Tables 1 and 2.

As shown in Tables 1 and 2, the encapsulating resin composition obtained by the method for producing the encapsulating resin composition of the example is different from the encapsulating resin composition obtained by the method for producing the encapsulating resin composition of the comparative example. Compared to encapsulant resin compositions, it has a lower coefficient of thermal expansion and higher hardness when heated, resulting in higher uniform dispersion of each component and higher mechanical properties and dimensional stability, which are practical physical properties. I understand that.

Claims (6)

preparing a dispersion containing an epoxy resin, a curing agent, an inorganic filler, a solvent, and an acetylene glycol compound;
a step of kneading the dispersion;
removing the solvent contained in the dispersion;
A method for producing a sealing resin composition having the following. The method for producing a sealing resin composition according to claim 1, wherein the acetylene glycol compound has an HLB value of 10 or less. A sealing resin composition containing an epoxy resin, a curing agent, an inorganic filler, and an acetylene glycol compound. The sealing resin composition according to claim 3, wherein the acetylene glycol compound has an HLB value of 10 or less. A method for producing an electronic component device, comprising the step of sealing an element with a sealing resin composition produced by the method for producing a sealing resin composition according to claim 1 or 2. Motoko and
A cured product of the sealing resin composition according to claim 3 or 4, which seals the element;
An electronic component device comprising: