JP2002003726A - Resin composition for sealing - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a resin composition for sealing use, exhibiting excellent sealing characteristics and producible without causing the problem of the abrasion of a kneader. SOLUTION: The resin composition for sealing contains 100 pts.wt. of a polymer resin and 100-900 pts.wt. of calcium carbonate.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sealing resin composition, and more particularly to a sealing material for electronic parts and devices.

[0002]

2. Description of the Related Art In recent years, with the remarkable development of the field of electronic engineering, conventional electronic components have been reduced in size and performance, and new electronic components and elements have been actively developed. When these components and elements are mounted on a device, sealing with a polymer resin material or a ceramic material is performed to maintain the reliability of the components and elements. According to the ceramic material, highly reliable sealing is possible,
Until now, high-performance parts have been used, but the manufacturing cost as a sealing material has been high. Therefore, recently, sealing with a general-purpose and inexpensive polymer resin material has become common.

In the case of a polymer resin sealing material, an inorganic filler is added to and mixed with the resin to improve the coefficient of thermal expansion and thermal conductivity of the sealing material. Conventionally, materials used as inorganic fillers are alumina and silica. However, since these materials have high hardness, problems such as abrasion of a kneader during kneading with a resin have occurred. Therefore, improvements such as imparting a certain shape to these materials (for example, spherical particles) have been required.

[0004]

Means for Solving the Problems The present inventors have conducted intensive studies in view of the above problems and as a result, have found a sealing resin composition using calcium carbonate as an inorganic filler instead of conventional alumina or silica. .

[0005] Calcium carbonate has excellent thermal stability, is stable up to about 500 ° C in the air, has excellent electrical insulation and dielectric properties as a sealing material, and has a lower hardness than alumina and silica. After repeated studies based on these facts, we solved the problem of wear caused when using alumina or silica by using a polymer resin composition using calcium carbonate as an inorganic filler as a sealing material. The inventors have found that the sealing material can be formed and that the cost is low, and the present invention has been completed.

That is, the present invention provides a sealing resin composition as described below. Item 1. 100 parts by weight of polymer resin and calcium carbonate 10
A sealing resin composition containing 0 to 900 parts by weight. Item 2. Polymer resin, epoxy resin, polyimide resin, polyurethane resin, phenolic resin, furan resin,
Item 2. The encapsulating resin composition according to item 1, wherein the resin composition is at least one selected from the group consisting of a melamine resin, a urea resin, a guanamine resin, a vinyl ester resin, an unsaturated polyester resin, and a diallyl phthalate resin. Item 3. BET specific surface area of calcium carbonate by nitrogen adsorption method is 15 m ² / g or less and average particle size is 1 to 70 μm
3. The encapsulating resin composition according to item 1 or 2, wherein the purity is 95% or more and the water content is 3.0% or less.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The term "resin composition for sealing" as used in the present invention means a resin composition mainly used for sealing electronic parts.

The polymer resin used in the present invention includes epoxy resins, polyimide resins, polyurethane resins, phenol resins, furan resins, melamine resins, urea resins, guanamine resins, vinyl ester resins, unsaturated polyester resins, diallyl phthalate resins and the like. Thermosetting resin,
Among them, epoxy resin, polyimide resin, polyurethane resin, phenol resin and furan resin are preferable. These resins are used alone or in combination of two or more.

[0009] BET specific surface area by nitrogen adsorption method of calcium carbonate used in the present invention is not more than 15 m ² / g, preferably 1~12m ² / g, more preferably 2 to
10 m ² / g. When the BET specific surface area by the nitrogen adsorption method exceeds 15 m ² / g, the primary particles of calcium carbonate are undesirably too fine. In the present invention,
Calcium carbonates having different specific surface areas may be mixed and used.

The average particle size of the calcium carbonate is 1 to 70.
μm, preferably 2 to 50 μm, more preferably 3 to 30 μm, particularly preferably 5 to 20 μm.
m. Here, the average particle size refers to a value obtained by a laser diffraction / scattering type particle size distribution measuring device. In the present invention, calcium carbonates having different average particle sizes may be mixed and used.

The purity of the above calcium carbonate is 95% or more, preferably 97 to 100%, more preferably 98 to 100%. When the purity is less than 95%,
When used as an inorganic filler, sufficient sealing properties may not be exhibited, which is not preferable. Purity here means
Refers to the value obtained in accordance with the official calcium carbonate purity test of food additives. In the present invention, calcium carbonates having different purities may be mixed and used.

The water content of the above calcium carbonate is 3.0% or less, preferably 0 to 1.5%, more preferably 0 to 1.0%. If the water content exceeds 3.0%, the resin may have a bad effect when mixed with the resin as an inorganic filler, which is not preferable. Here, the water content refers to a value obtained by a moisture test method for chemical products according to JIS K 0068. In the present invention, calcium carbonates having different moisture contents may be mixed and used.

The method for producing the above calcium carbonate is not particularly limited, but a method of pulverizing limestone (heavy calcium carbonate) or a method of calcining limestone and reacting with water to form calcium hydroxide, and then producing carbon dioxide gas (Precipitable calcium carbonate) is preferred. Further, these calcium carbonates having different production methods can be used in combination.

The shape of the calcium carbonate particles may be any of a granular shape, a plate shape, a columnar shape, a needle shape and a cubic shape. Particles having a granular or cubic shape are preferred from the viewpoint of flowability. Particles having a plate-like, columnar or needle-like shape are preferred from the viewpoint of improving the mechanical strength and the like of the resin composition. Therefore, a resin composition having desired characteristics can be obtained by mixing and using particles having different shapes.

As the crystal form of the calcium carbonate, calcite, badderite, aragonite, or amorphous is known, but is not particularly limited in the present invention.

In producing the encapsulating resin composition of the present invention, the surface treatment of the calcium carbonate particles using a surface treating agent can improve the compatibility with the resin. Examples of effective surface treatment agents include fatty acids, rosins, Teflon (registered trademark), silicones, modified silicones, and silane coupling agents. For example, fatty acids include, specifically, stearic acid, oleic acid, and the like, and silane coupling agents include vinyl silane, amino silane, epoxy silane, chloroalkyl silane, mercapto silane, methyl triethoxy silane, and the like. . The coating amount of these surface treatment agents varies depending on the resin and application, but is preferably 0.01 to 10% by weight, more preferably 0.05 to 7% by weight, and particularly preferably 0.5 to 5% by weight based on calcium carbonate. 5% by weight. If the ratio is out of this range, the surface treatment effect may not be exhibited, or the compatibility with the resin may be deteriorated, and it may be difficult to obtain desired viscosity characteristics and the like in the obtained resin composition, which is not preferable.

The surface treatment method is not particularly limited as long as the surface of the calcium carbonate particles can be coated with the surface treatment agent, and a known method can be used. For example, coating can be performed by preparing a slurry of calcium carbonate in advance, mixing a surface treatment agent with the slurry, and mixing and kneading. Alternatively, the calcium carbonate powder can be coated by directly spraying a liquefied surface treatment agent.

The content of calcium carbonate in the resin composition of the present invention is 100 to 9 parts by weight per 100 parts by weight of the resin.
00 parts by weight, preferably 150 to 700 parts by weight, more preferably 200 to 500 parts by weight. If the content of calcium carbonate is less than 100 parts by weight, it is difficult to improve the properties of the resin. On the other hand, if it exceeds 900 parts by weight, it becomes difficult for the resin to cover the calcium carbonate uniformly, and it is difficult to obtain a good sealing resin composition.

The resin composition of the present invention may contain an inorganic filler other than calcium carbonate as long as the effects of the present invention are not impaired. Such inorganic fillers include alumina, silica, magnesia, magnesia-alumina spinel, beryllia, mullite, zinc oxide, boron nitride, aluminum nitride, silicon nitride, silicon carbide, boron carbide, zeolite, talc, bentonite, kaolin, etc. Is mentioned. The content ratio of these varies depending on the type of the inorganic filler, but is preferably 0 to 50% by weight, more preferably 0 to 30% by weight, and particularly preferably 0 to 20% by weight of the content of calcium carbonate.

The mixing of the resin and the inorganic filler at the time of producing the encapsulating resin composition of the present invention is not particularly limited, and is performed by a generally used mixing apparatus and mixing method.

[0021]

The sealing resin composition of the present invention uses calcium carbonate as an inorganic filler to reduce the abrasion of a kneading machine which has conventionally been a problem in the production of resin compositions containing alumina and silica. Eliminate problems. In addition, the sealing resin composition of the present invention has thermal conductivity, electrical insulation, dielectric properties, and a pressure cooker test, which are equal to or higher than the sealing resin composition containing alumina or silica. Is shown. Furthermore, since calcium carbonate is a cheaper material than alumina and silica, the present invention is very useful in the field of electronic materials.

[0022]

The present invention will be described in more detail with reference to the following Examples, which by no means limit the present invention.

Example 1 A BET specific surface area measured by a nitrogen adsorption method was 5 m ² / g, and an average particle diameter measured by a laser diffraction / scattering type particle size distribution analyzer was 15%.
The purity determined in accordance with the calcium carbonate purity test of the official standard of food additives was 98.0% in JIS K 006 μm.
The surface of a heavy calcium carbonate powder having a moisture content of 0.6% according to the moisture test method of Chemical Product No. 8 was treated with a silane coupling agent (epoxysilane) (coating amount: 1.0% by weight).

The surface-treated calcium carbonate (350 parts by weight) and epoxy resin (trade name "KMC" manufactured by Shin-Etsu Chemical Co., Ltd.)
-130 ") was sufficiently mixed with a kneader to obtain a resin composition. At that time, no abrasion of the kneader was observed. When the obtained resin composition was used as a sealing resin composition for a semiconductor element component, good sealing properties were exhibited.

Example 2 BE in a calcium hydroxide slurry by a nitrogen adsorption method
Calcium carbonate powder having a T specific surface area of 10 m ² / g and an average particle size of 2 μm was added, and carbon dioxide was blown into the slurry to precipitate calcium carbonate. The obtained calcium carbonate is further added to a calcium hydroxide slurry,
Calcium carbonate was precipitated by the same operation. By repeating this operation, the BET specific surface area by the nitrogen adsorption method is 4 m ² / g, the average particle size by the laser diffraction scattering type particle size distribution measuring device is 10 μm, and it conforms to the official calcium carbonate purity test of food additives. Purity determined by the above.
At 0%, a calcium carbonate powder having a moisture content of 0.5% according to the moisture test method for chemical products according to JIS K 0068 was obtained. This powder was surface-treated using a silane coupling agent (methyltriethoxysilane) solution (coating amount: 1.5% by weight).

The obtained surface-treated calcium carbonate powder is
It was mixed with an epoxy resin in the same manner as in Example 1, and a reliability test was performed. As a result, good sealing characteristics were exhibited as the sealing resin composition, and no abrasion of the kneader during mixing was observed.

Example 3 A calcium carbonate having a BET specific surface area of 15 m ² / g and an average particle size of 0.5 μm as a seed by a nitrogen adsorption method was added to a calcium hydroxide slurry, and carbon dioxide gas was blown into the calcium hydroxide slurry. Calcium carbonate was precipitated. Using the obtained calcium carbonate as a seed,
By repeating the same operation, B by nitrogen adsorption method
The ET specific surface area is 10 m ² / g, the average particle size by a laser diffraction scattering type particle size distribution analyzer is 5 μm, and the purity determined according to the calcium carbonate purity test of the official standard of food additives is 98.5%. A calcium carbonate powder having a moisture content of 1.0% according to the moisture test method for chemical products according to JIS K 0068 was obtained. This powder was surface-treated using a fatty acid-based surface treatment agent (stearic acid) (coating amount: 3.0% by weight).

This surface-treated calcium carbonate (400 parts by weight) and a polyimide resin (trade name "TI-300" manufactured by Toray Industries, Inc.) are used.
0 ") and 100 parts by weight were sufficiently mixed by a kneader to obtain a resin composition. At that time, no abrasion of the kneader was observed. Using the obtained resin composition as a sealing material for a semiconductor element part, a reliability test was performed, and good results were obtained.

Example 4 The mixed powder obtained by mixing the calcium carbonate powders obtained in Examples 2 and 3 at a weight ratio of 1: 1 was mixed with a fatty acid-based surface treating agent (stearic acid). (Coating amount: 3.0% by weight).

The surface treated calcium carbonate (350 parts by weight) and a phenol resin (trade name "NAIS" manufactured by Matsushita Electric Works, Ltd.)
-CY6051 ") was sufficiently mixed with a kneader to obtain a resin composition. At that time, no abrasion of the kneader was observed. Using the obtained resin composition as a sealing material for a semiconductor element component, a reliability test was performed. As a result, good sealing characteristics were obtained.

Comparative Example 1 A resin composition was obtained in the same manner as in Example 1 except that alumina powder having an average particle size of 5 μm was used instead of heavy calcium carbonate powder. At the time of mixing, abrasion of the kneader was observed, and the iron content in the obtained resin composition was significantly increased.

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Claims (3)

[Claims] 1. A sealing resin composition containing 100 parts by weight of a polymer resin and 100 to 900 parts by weight of calcium carbonate. 2. The polymer resin is selected from the group consisting of epoxy resin, polyimide resin, polyurethane resin, phenol resin, furan resin, melamine resin, urea resin, guanamine resin, vinyl ester resin, unsaturated polyester resin and diallyl phthalate resin. The sealing resin composition according to claim 1, wherein the resin composition is at least one selected from the group consisting of: 3. BE by calcium carbonate nitrogen adsorption method
T specific surface area is 15m ^Two/ G or less and an average particle size of 1 to 70
μm, purity is 95% or more, and water content is 3.0% or more
The seal according to claim 1 or 2, wherein the seal is below.
A resin composition for stopping.