JP6458462B2 - Method for producing thermosetting resin composition, and thermosetting resin composition obtained thereby - Google Patents

Description

  The present invention relates to a method for producing a thermosetting resin composition used for an electronic component, and a thermosetting resin composition obtained thereby.

  In semiconductor packages, thermosetting resin compositions such as epoxy resins containing inorganic fillers are widely used as sealing materials for protecting semiconductor elements from the environment. The inorganic filler added to the thermosetting resin lowers the thermal expansion coefficient of the thermosetting resin, suppresses the warpage of the resin cured product, and prevents the occurrence of interface peeling and cracks in the semiconductor package.

  Since the adhesion between the inorganic filler and the thermosetting resin is poor if the raw material is intact, the surface of the inorganic filler is surface-treated before mixing with the thermosetting resin main component.

  For example, Patent Document 1 includes a step of heating a granular silica at a temperature of 100 ° C. to 1000 ° C. for 1 hour to 24 hours to reduce silanol groups present on the surface of the granular silica, and a silane coupling treatment. A method for producing a silica filler is disclosed, including a step of performing.

  Patent Document 2 discloses (A) an epoxy resin, (B) a phenol resin as a curing agent, (C) an inorganic filler, and (D) (a) an aluminum chelate compound and (b) a diazabicycloalkene and its derivatives. And an epoxy resin composition containing a silane coupling agent in which at least one compound is dissolved as an essential component. And it comprises the inorganic filler of (C) surface-treated with the silane coupling agent of (D) at a ratio of 25 to 95% by weight with respect to the entire resin composition.

Japanese Patent Laid-Open No. 11-43320 Japanese Patent Laid-Open No. 10-287796

  However, when the inorganic filler is surface-treated with a silane coupling agent, the thermosetting resin is hydrolyzed by unreacted silanol groups introduced by the silane coupling agent. Therefore, heat resistance and moisture resistance are lowered, which is not preferable in terms of improving the reliability of the semiconductor package.

  Therefore, an object of the present invention is to improve the adhesion between the inorganic filler and the thermosetting resin, and to obtain a cured product having excellent heat resistance and moisture resistance, and a method for producing a thermosetting resin composition, thereby It is in providing the thermosetting resin composition obtained and the electronic component using this thermosetting resin composition.

In order to achieve the above object, the method for producing a thermosetting resin composition of the present invention comprises a step of removing organic substances from the surface of an inorganic filler to obtain a clean surface, and an aluminum chelate on the clean surface of the inorganic filler. compounds, titanium chelate compounds, one selected from zirconium chelate compound or a step of depositing a chelate compound is 2 or more, the inorganic filler was deposited with the chelating compound and dried in the chelating compound Including a step of obtaining the coated inorganic filler, and a step of adding and mixing a thermosetting resin composition as a main agent and a curing agent to the inorganic filler coated with the chelate compound. Features.

The thermosetting resin composition of the present invention comprises a thermosetting resin as a main agent, a curing agent for curing the thermosetting resin , an inorganic filler having a clean surface from which organic substances are removed from the surface, and the inorganic And a chelate compound that is one or more selected from an aluminum chelate compound, a titanium chelate compound, and a zirconium chelate compound that covers the clean surface of the filler.

  The electronic component of the present invention is characterized in that a sealing material obtained by curing the thermosetting resin composition according to the present invention described above is used at least in part.

According to the present invention, the adhesion between the inorganic filler and the thermosetting resin is improved through the chelate compound by depositing the chelate compound after removing organic substances from the surface of the inorganic filler to obtain a clean surface. To do. Therefore, a thermosetting resin composition excellent in moisture resistance and heat resistance can be produced. And by using this thermosetting resin composition as a sealing material for an electronic component, the heat resistance and moisture resistance of the sealing material can be improved, and the reliability of the electronic component can be increased. In particular, it can be suitably used for electric / power devices such as automobiles, vehicles, aircraft, ships, vending machines, air conditioners, and generators that are difficult to manage the environment and are used outdoors.

The thermosetting resin composition of the embodiment of the present invention includes a thermosetting resin as a main agent, a curing agent, and an inorganic filler coated with a chelate compound . With these components, a cured product having high adhesion between the thermosetting resin and the inorganic filler and excellent in moisture resistance and heat resistance can be provided. Hereinafter, each of these constituent requirements will be described more specifically.

  It does not specifically limit as a thermosetting resin used for this embodiment, For example, an epoxy resin, a phenol resin, a maleimide resin etc. can be mention | raise | lifted. Among them, an epoxy resin having at least two epoxy groups in one molecule is particularly preferable for use in electronic components because of its high dimensional stability, water resistance / chemical resistance and electrical insulation. Specifically, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol E type epoxy resin, bisphenol S type epoxy resin, bisphenol AD type epoxy resin, naphthalene type epoxy resin, phenol novolac type epoxy resin, cresol novolak type epoxy resin And maleimide naphthol resin, maleimide triazine resin, maleimide resin, glycidyl ester type epoxy resin, and glycidyl amine type epoxy resin. These thermosetting resins may be used alone or in combination of two or more. Depending on the combination to be copolymerized, physical properties such as heat resistance, toughness and flame retardancy can be appropriately adjusted. Moreover, in order to adjust a viscosity and a crosslinking density, the reactive diluent which has crosslinking | crosslinked functional groups, such as an epoxy group, can be mixed with a thermosetting resin suitably.

  The curing agent used in the present embodiment is not particularly limited, and for example, an aromatic acid anhydride, specifically, phthalic anhydride, pyromellitic anhydride, trimellitic anhydride, or a cyclic aliphatic acid anhydride, Specifically, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl nadic anhydride, etc., or aliphatic acid anhydrides, specifically succinic anhydride, polyadipic acid An anhydride, a poly sebacic acid anhydride, a poly azelaic acid anhydride etc. can be mentioned.

  In the above, tertiary amine, boric acid ester, Lewis acid, organic metal compound, organic acid metal salt, triphenylphosphine, imidazole and the like can be appropriately blended as a curing accelerator.

  Examples of the inorganic filler used in the present embodiment include fused silica, silica, alumina, aluminum hydroxide, talc, clay, mica, and glass fiber. This is because these inorganic fillers can increase the thermal conductivity of the cured product and reduce the thermal expansion coefficient. These inorganic fillers may be used alone or in combination of two or more.

As the chelate compound used in this embodiment, for example, a solution diluted by adding a diluting solvent to one or more selected from an aluminum chelate compound, a titanium chelate compound, and a zirconium chelate compound is preferable. This is because these chelate compounds can form a film on the surface of the inorganic filler and can effectively enhance the adhesion to the thermosetting resin.

  Specific examples of the aluminum chelate compound include aluminum ethyl acetoacetate diisopropylate, diethoxy mono (acetylacetonato) aluminum, di-n-propoxy mono (acetylacetonato) aluminum, and di-i-propoxy mono. (Acetylacetonato) aluminum, di-n-butoxy mono (acetylacetonato) aluminum, di-sec-butoxy mono (acetylacetonato) aluminum, di-t-butoxy mono (acetylacetonato) aluminum, ethoxy -Bis (acetylacetonate) aluminum is mentioned.

  Specific examples of the titanium chelate compound include titanium diisopropoxybis (ethylacetoacetate), triethoxy mono (acetylacetonato) titanium, tri-n-propoxymono (acetylacetonato) titanium, tri-i. -Propoxy mono (acetylacetonato) titanium, tri-n-butoxy mono (acetylacetonato) titanium, tri-sec-butoxy mono (acetylacetonato) titanium, tri-t-butoxy mono (acetylacetonate) ) Titanium, diethoxy bis (acetylacetonato) titanium, di-n-propoxy bis (acetylacetonato) titanium, zi-propoxy bis (acetylacetonato) titanium, di-n-butoxy bis (acetylacetate) NAART) Titanium That.

  Zirconium chelate compounds are zirconium dibutoxybis (ethylacetoacetate), triethoxy mono (acetylacetonato) zirconium, tri-n-propoxy mono (acetylacetonato) zirconium, tri-i-propoxy mono (acetyl) Acetonato) zirconium, tri-n-butoxy mono (acetylacetonato) zirconium, tri-sec-butoxymono (acetylacetonato) zirconium, tri-t-butoxymono (acetylacetonato) zirconium, diethoxy bis (Acetylacetonato) zirconium, di-n-propoxy bis (acetylacetonato) zirconium, zi-propoxy bis (acetylacetonato) zirconium.

  As a solvent for diluting the chelate compound, alcohol solvents, specifically N-methyl-2-pyrrolidone, methanol ethanol 1-propanol, isopropanol, 1-butanol, or aromatic solvents, specifically toluene, xylene , Cumene, or amide solvents, specifically N, N-dimethylacetamide, N, N-dimethylformamide, or lactone solvents, specifically γ-butyrolactone, γ-valerolactone, or glycol solvents, specifically Specifically, methyl cellosolve, ethyl cellosolve, propylene glycol monomethyl ether acetate and the like can be mentioned, and one or more can be used.

  Next, the blending amount of each component will be described based on 100 parts by mass of a thermosetting resin (including a reactive diluent) that is a main component.

  As for the compounding quantity of a hardening | curing agent, 50-150 mass parts is preferable with respect to 100 mass parts of thermosetting resins which are main ingredients. When the blending amount of the curing agent is less than 50 parts by mass, the glass transition temperature is lowered due to insufficient crosslinking, and when it exceeds 150 parts by mass, moisture resistance, high heat distortion temperature, and heat stability are deteriorated.

  As for the compounding quantity of an inorganic filler, 200-600 mass parts is preferable with respect to 100 mass parts of thermosetting resins which are the main ingredients. When the blending amount of the inorganic filler is less than 200 parts by mass, the thermal expansion coefficient of the sealing material is increased and peeling and cracking are likely to occur, and the viscosity of the composition having a blending amount greater than 600 parts by mass increases. Extrudability deteriorates.

As for the compounding quantity of a chelate compound , 0.1-3 mass parts is preferable with respect to 100 mass parts of thermosetting resins which are the main ingredients. When the compounding amount of the chelate compound is less than 0.1 parts by mass , the coating of the chelate compound on the surface of the inorganic filler is not sufficient, resulting in poor adhesion, and when the compounding amount is more than 3 parts by mass, the glass transition temperature is remarkably lowered. Therefore, it is not preferable.

By mix | blending an inorganic filler as mentioned above, the heat conductivity of hardened | cured material can be improved and a thermal expansion coefficient can be reduced. Moreover, a film | membrane is uniformly formed on the surface of an inorganic filler by mix | blending a chelate compound as mentioned above, and the adhesiveness of an inorganic filler and a thermosetting resin can be improved effectively.

  Next, the manufacturing method of the thermosetting resin composition of embodiment of this invention is demonstrated.

The manufacturing method of the thermosetting resin composition of the present embodiment,
(Step 1) A step of removing organic substances from the surface of the inorganic filler to obtain a clean surface;
(Step 2) depositing a chelate compound on the clean surface of the inorganic filler;
(Step 3) drying the chelate compound an inorganic filler is deposited and a step of obtaining an inorganic filler coated with a chelate compound,
(Step 4) A step of adding a thermosetting resin as a main agent and a curing agent to an inorganic filler coated with a chelate compound and mixing them is included. According to this production method, the organic substance is removed from the surface of the inorganic filler to form a clean surface, and then the chelate compound is deposited, whereby the adhesion between the inorganic filler and the thermosetting resin is achieved via the chelate compound. improves. Therefore, a thermosetting resin composition excellent in moisture resistance and heat resistance can be produced.

  In step 1, the surface of the inorganic filler is cleaned. As the cleaning method, for example, oxygen plasma treatment and ultraviolet irradiation treatment are preferably employed.

The oxygen plasma treatment is a surface treatment method in which fine powder of an inorganic filler is exposed to oxygen plasma in a plasma apparatus. Since the organic substance on the surface of the inorganic filler can be decomposed and removed by the chemical action of oxygen radicals and oxygen ions contained in the oxygen plasma, the surface of the inorganic filler can be cleaned. Therefore, the alkoxy group of the chelate compound and the hydroxyl group of the inorganic filler are chemically bonded, and the adhesion with the thermosetting resin can be enhanced. The plasma apparatus to be used is not particularly limited, and for example, a parallel plate type plasma apparatus, a barrel type plasma apparatus, a remote type plasma apparatus, or the like can be used. On the other hand, in an apparatus of a type that performs plasma processing under reduced pressure, fine powder of an inorganic filler may be scattered during evacuation, so an atmospheric pressure plasma apparatus that can perform plasma processing even at atmospheric pressure is preferable. Atmospheric pressure plasma can be generated by corona discharge, dielectric barrier discharge, glow discharge, or microwave discharge. For example, according to a method in which fine powder of an inorganic filler is placed on a belt conveyor and passed under a plasma source, continuous processing is possible, and mass productivity is excellent.

On the other hand, the ultraviolet irradiation treatment is a surface treatment method in which fine powder of an inorganic filler is exposed to ozone generated by ultraviolet irradiation. And since the organic substance on the surface of the inorganic filler can be decomposed and removed by the chemical action of the generated ozone, the surface of the inorganic filler can be cleaned. Therefore, the alkoxy group of the chelate compound and the hydroxyl group of the inorganic filler are chemically bonded, and the adhesion with the thermosetting resin can be enhanced. The ultraviolet irradiation treatment may be a batch type, but may be a continuous treatment in which a fine powder of an inorganic filler is placed on a belt conveyor and passed under an ultraviolet lamp.

The surface cleaned by the oxygen plasma treatment or the ultraviolet irradiation treatment is excellent in wettability and can uniformly deposit the chelate compound .

In step 2, a chelate compound is deposited on the surface of the inorganic filler. As the deposition method, for example, a spray treatment of the chelate solution or an immersion treatment in the chelate solution is preferably employed.

The spray treatment is a method in which a chelate compound is deposited on the surface of the inorganic filler by spraying a predetermined amount of the chelate solution over time while stirring the powder of the inorganic filler in a stirring tank. By the spray treatment, the chelate compound can be uniformly deposited on the surface of the cleaned inorganic filler. As a stirrer, a Henschel mixer, a Laedige mixer, or the like can be used. The concentration of the chelate solution is preferably 30 to 70% by mass. If the concentration of the chelating solution is lower than 30% by mass, the working efficiency is poor, and if it is higher than 70% by mass, adhesion spots occur, which is not preferable. Further, if the spraying speed is too high, it is not preferable because deposition spots occur. Usually, spraying is performed for several tens of minutes. According to the spraying process, the amount of solvent used can be saved. Since the solvent volatilizes more and more during the spraying operation, it is possible to save the trouble of subsequent solid-liquid separation.

On the other hand, the dipping treatment is a method in which the powder of the inorganic filler is put into a stirring tank together with the chelate solution, stirred for a predetermined time, and the chelate compound is deposited on the surface of the inorganic filler. According to the immersion treatment, the chelate compound can be more uniformly deposited on the surface of the cleaned inorganic filler as compared with the spray treatment.

In step 3, for example, excess solvent is volatilized in a drying furnace. By this step, a uniform film of the chelate compound can be formed on the surface of the inorganic filler. For example, the drying can be performed with hot air at 120 ° C. for 30 minutes.

In step 4, the inorganic filler coated with the chelate compound , the thermosetting resin as the main agent, and the curing agent are uniformly mixed using a kneader. Thereby, the thermosetting resin composition of this embodiment is obtained.

  The thermosetting resin composition of the present invention thus obtained can be used as, for example, a sealing material for electronic components, an insulating material, a substrate material, a mounting material, and the like. For example, when used as a sealing material for electronic components, a semiconductor element may be placed in a mold together with a lead frame, and a thermosetting resin may be injection molded into the gap. Since the thermosetting resin composition of the present invention is excellent in heat resistance and moisture resistance after becoming a curable resin, by using it as a sealing material for electronic components, a semiconductor element can be removed from the surrounding environment over a long period of time. The excellent effect of protecting is brought about. Therefore, it can be suitably used for applications such as automobiles that require high reliability.

  Hereinafter, the present invention will be described in more detail with reference to examples.

[Example 1]
(Process 1)
A fused silica having an average particle size of 5 μm (manufactured by Ashimori Co., Ltd., trade name “ZA-30”) was placed on a processing table of a plasma processing apparatus PD-2203L manufactured by Samco and evacuated, and then oxygen was introduced. The plasma treatment was performed at a power of 200 W for 3 minutes.

(Process 2)
520 parts by mass of oxygen plasma-treated fused silica is charged into a Henschel mixer, and 0.2 parts by mass of aluminum ethyl acetoacetate diisopropylate (ALCH manufactured by Kawaken Fine Chemical Co., Ltd.) is added while the fused silica is being stirred. The chelating solution was sprayed.

(Process 3)
Chelate-treated 520 parts by mass of fused silica was dried with hot air at 120 ° C. for 3 minutes.

(Process 4)
To 520 parts by mass of the fused silica obtained in step 3, 50 parts by mass of bisphenol A type epoxy resin (manufactured by Nippon Steel & Sumikin Co., Ltd., trade name “YD-825GS”), aminoglycidyl ether type epoxy resin (manufactured by Japan Epoxy Resin Co., Ltd.) , Trade name EP-630) 100 parts by mass of an epoxy resin main component composed of 30 parts by mass, 20 parts by mass of a reactive diluent, 120 parts by mass of an acid anhydride, and 1 part by mass of a curing accelerator, A curable resin composition was obtained.

(Process 5)
The thermosetting resin composition was poured into a mold, heated at 100 ° C. for 1 hour, and further heated at 170 ° C. for 1 hour to be cured.

[Example 2]
In the process 2 of Example 1, the chelate solution which mix | blended 0.5 mass part of aluminum ethyl acetoacetate diisopropylate was sprayed. Other steps were in accordance with the method of Example 1.

[Example 3]
In Step 2 of Example 1, a chelate solution containing 1.0 part by mass of aluminum ethyl acetoacetate diisopropylate was sprayed. Other steps were in accordance with the method of Example 1.

[Example 4]
In Step 2 of Example 1, a chelate solution containing 0.5 parts by mass of titanium diisopropoxybis (ethyl acetoacetate) was sprayed. Other steps were in accordance with the method of Example 1.

[Example 5]
In the process 2 of Example 1, the chelate solution which mix | blended 0.5 mass part of zirconium dibutoxybis (ethyl acetoacetate) was sprayed. Other steps were in accordance with the method of Example 1.

[Comparative Example 1]
A thermosetting resin composition obtained by kneading 520 parts by mass of fused silica, 100 parts by mass of the epoxy resin main component of Example 1, 120 parts by mass of an acid anhydride, and 1 part by mass of a curing accelerator was obtained using gold. After pouring into a mold and heating at 100 ° C. for 1 hour, it was further cured by heating at 170 ° C. for 1 hour.

[Comparative Example 2]
520 parts by weight of fused silica coated with 0.25 parts by weight of a silane coupling agent γ-glycidoxypropyltrimethoxysilane, 100 parts by weight of the epoxy resin main agent of Example 1, 120 parts by weight of an acid anhydride, A thermosetting resin composition obtained by kneading 1 part by mass of a curing accelerator was poured into a mold, heated at 100 ° C. for 1 hour, and further cured by heating at 170 ° C. for 1 hour.

[Comparative Example 3]
520 parts by mass of fused silica coated with 0.5 parts by mass of a silane coupling agent γ-glycidoxypropyltrimethoxysilane, 100 parts by mass of the epoxy resin main agent of Example 1, and 120 parts by mass of an acid anhydride, A thermosetting resin composition obtained by kneading 1 part by mass of a curing accelerator was poured into a mold, heated at 100 ° C. for 1 hour, and further cured by heating at 170 ° C. for 1 hour.

[Comparative Example 4]
520 parts by mass of fused silica coated with 1.0 part by mass of a silane coupling agent γ-glycidoxypropyltrimethoxysilane, 100 parts by mass of the epoxy resin main agent of Example 1, 120 parts by mass of acid anhydride, A thermosetting resin composition obtained by kneading 1 part by mass of a curing accelerator was poured into a mold, heated at 100 ° C. for 1 hour, and further cured by heating at 170 ° C. for 1 hour.

[Comparative Example 5]
In the method of Example 1, the oxygen plasma treatment in Step 1 was omitted. Other steps were in accordance with the method of Example 1.

  Hereinafter, a method for evaluating a thermoset will be described.

[Adhesive strength]
The Cu plate was cut into a 10 mm square shape and a fluororesin mold was fixed. The resin was poured and heated at 100 ° C. for 1 hour, and further heated at 170 ° C. for 1 hour to form a cured product having an adhesion area of 10 mm ² , an upper surface of 3 mm, and a height of 4 mm on the Cu plate. This cured product was pressed at 1 mm / sec in parallel with the copper circuit foil surface, and the maximum breaking load was measured. The test was performed at each n = 5, and the load measurement value per unit bonding area was defined as adhesion strength.

[Glass-transition temperature]
Using a thermomechanical analysis (TMA) apparatus TMA / SS7100 manufactured by SII, a curve indicating the relationship between the resin temperature and the amount of thermal deformation was measured, and the inflection point was defined as the glass transition temperature.

[Elastic modulus]
Using a universal material testing apparatus (AG-50kNX) manufactured by Shimadzu Corporation, the strain against stress was measured, and the inclination was defined as the elastic modulus.

[Thermal expansion coefficient]
Using a thermomechanical analysis (TMA) apparatus TMA / SS7100 manufactured by SII, the amount of change in length with respect to the resin temperature was measured, and the slope before the inflection point was defined as the linear expansion coefficient.

[Water absorption rate]
The water absorption rate of the cured product was calculated from the mass change before and after being left at high temperature and high humidity (temperature 85 ° C., relative humidity 85%, 1000 hours).

Water absorption [%] = (W2-W1) / W1 × 100 (1)
Here, W1 represents the sample mass before the test, and W2 represents the sample mass before the test.

[Defect rate]
After ten test devices sealed with the thermosetting resin composition obtained in the examples were left at high temperature and high humidity (temperature 85 ° C., relative humidity 85%, 1000 hours), electrical characteristics (open, leaked) Etc.) and the number of defects was expressed as a percentage.

  Hereinafter, the evaluation results will be described.

  Table 1 shows the results of evaluating the adhesiveness by changing the surface treatment method.

  First, mechanical strength is compared. The epoxy resin cured product (Example 2) using silica treated with aluminum chelate after oxygen plasma treatment as a filler (Example 2) has an adhesive strength of about twice as good as that of the conventional cured product of silane coupling treatment (Comparative Example 3). It is. However, when the oxygen plasma treatment was not performed (Comparative Example 5), the adhesion strength was remarkably reduced, and the effect of the aluminum chelate treatment was not observed.

  Although the titanium chelate treatment (Example 4) and the zirconium chelate treatment (Example 5) do not reach the effect of the aluminum chelate treatment (Example 2), the conventional cured product obtained by silane coupling treatment (Comparative Example 3). Also has excellent adhesion strength.

Therefore, an aluminum chelate compound, a titanium chelate compound, and a zirconium chelate compound are effective as treatment agents that are deposited on the silica surface to improve the adhesion between the silica and the epoxy resin and increase the adhesion strength to the Cu substrate. Aluminum chelate compounds are excellent. However, it is necessary to clean the silica surface by oxygen plasma treatment before the aluminum chelate treatment in order to increase the mechanical strength.

Next, the glass transition temperature will be compared. An epoxy resin cured product (comparative example 4) containing silica sprayed with 1 part by mass of a silane coupling agent as a filler (Comparative Example 4) is a cured epoxy resin product containing silica sprayed with 0.25 parts by mass of a silane coupling agent ( The glass transition temperature is lower than in Comparative Example 2). However, in the case of an aluminum chelate compound, the glass transition temperature hardly decreases even when 1 part by mass is sprayed.

Therefore, the heat resistance of the cured product can be increased by using silica sprayed with an aluminum chelate compound after oxygen plasma treatment as a filler.

Regarding the elastic modulus and thermal expansion coefficient, no significant difference was observed between the case of using the aluminum chelate compound and the case of using the silane coupling agent, and they were almost the same.

  The water absorption after standing at high temperature and high humidity is the cured epoxy resin with the untreated silica as the filler (Comparative Example 1) and the cured epoxy resin with the silica treated with the silane coupling (Comparative Examples 2 and 4). ), The epoxy resin cured product (Examples 1, 2, and 3) using aluminum chelate-treated silica as a filler is almost halved.

Therefore, the moisture resistance of the cured product can be enhanced by using silica sprayed with an aluminum chelate compound after oxygen plasma treatment as a filler.

  The defect rate after leaving at high temperature and high humidity is as follows: epoxy resin-encapsulated parts using untreated silica as a filler (Comparative Example 1), epoxy resin-encapsulated parts using silane-coupled silica as a filler (Comparative Example 2) 4) is 100%, but it is 0% in the epoxy resin encapsulated parts (Examples 1, 2 and 3) using silica treated with aluminum chelate as a filler.

Therefore, the reliability of the epoxy resin-encapsulated component can be improved by using silica sprayed with an aluminum chelate compound after oxygen plasma treatment as a filler.

As described above, when silica that has been subjected to oxygen plasma treatment and then sprayed with an aluminum chelate compound is used as a filler, it is possible to improve the adhesion between silica and epoxy resin, and to obtain a highly reliable electronic component with excellent heat resistance and moisture resistance. .

Claims (11)

Removing organic substances from the surface of the inorganic filler to obtain a clean surface;
A step of depositing the aluminum chelate compound to the clean surface of the inorganic filler, a titanium chelate compound, chelate compound is one or more selected from zirconium chelate compound,
A step of obtaining the chelate compound the inorganic filler is deposited is dried the inorganic filler coated with the chelating compound,
Adding and mixing the thermosetting resin as the main agent and the curing agent to the inorganic filler coated with the chelate compound ;
The manufacturing method of the thermosetting resin composition characterized by including.   The method for producing a thermosetting resin composition according to claim 1, wherein the method for removing organic substances from the surface of the inorganic filler is oxygen plasma treatment.   The method for producing a thermosetting resin composition according to claim 1, wherein the method for removing organic substances from the surface of the inorganic filler is ultraviolet irradiation. How to deposit the chelating compound to the clean surface of the inorganic filler, a solution prepared by diluting the chelate compound in a solvent, any one of claims 1 to 3 is a method of spraying the cleaning surface of the inorganic filler The manufacturing method of the thermosetting resin composition as described in one. How to deposit the chelating compound to the clean surface of the inorganic filler, the chelate compound solution diluted with a solvent, in the any one of claims 1 to 3 is a method of immersing the inorganic filler The manufacturing method of the thermosetting resin composition of description. A thermosetting resin as the main agent,
A curing agent for curing the thermosetting resin;
An inorganic filler having a clean surface from which organic substances have been removed from the surface;
Covering the clean surface of the inorganic filler, and an aluminum chelate compound, titanium chelate compound, chelate compound is one or more selected from zirconium chelate compound,
The thermosetting resin composition characterized by having. The thermosetting resin composition according to claim 6, wherein a maximum breaking load per unit bonding area with respect to the Cu material is 12.4 to 19.3 MPa. The thermosetting resin composition according to claim 6 or 7, wherein the water absorption is 0.43 to 0.49%. The thermosetting resin composition according to any one of claims 6 to 8, wherein a blending amount of the inorganic filler is 200 to 600 parts by mass with respect to 100 parts by mass of the thermosetting resin. object. Wherein the inorganic filler is fused silica, silica, alumina, aluminum hydroxide, talc, clay, mica, into any one of claims 6 to 9 is one or a mixture of two or more selected from glass fibers The thermosetting resin composition as described. Any sealing material to cure the thermosetting resin composition according to one the electronic components used in at least a portion of the claims 6-10.