JPS6162516A - Resin composition for sealing semiconductor - Google Patents

Abstract

PURPOSE:To provide the titled composition having excellent moisture resistance, high-temperature electrical characteristics, mold-releasability, etc. and giving a molded article having high printability, by adding a specific amount of a specific dibasic fatty acid bisamide compound as an internal releasing agent to an epoxy resin. CONSTITUTION:The objective composition can be prepared by compounding (A) an epoxy resin with (B) 0.01-10wt% internal releasing agent consisting of a dibasic fatty acid biasamide of formula (l and n is >=14; m is >=3) (prefer ably a condensation product of a >=5C dibasic fatty acid and >=15C long-chain aliphatic primary amine, and having a melting point of 80-140 deg.C).

Description

[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a semiconductor encapsulating resin composition for encapsulating a semiconductor element. It relates to a resin composition for semiconductor encapsulation that has excellent release properties during molding and also has good marking properties on the resulting molded products.

[Prior art]

Conventionally, the verme-cutter method using metals, ceramics, etc. has been used as a encapsulation technology for semiconductor elements, but resin encapsulation has become more economical in terms of productivity and cost, so resin encapsulation has become popular in recent years. It is becoming mainstream.

Epoxy resins for low-pressure molding, which can be suitable for low-pressure transfer molding, are widely used as resins for semiconductor encapsulation.

In such a transfer molding method, in order to enable the molded semiconductor to be removed from the mold, it is a common practice to add an internal mold release agent to the epoxy resin composition in advance. Conventionally commonly used internal mold release agents include long chain fatty acids such as stearic acid, metal salts of long chain fatty acids such as zinc stearate, ester waxes of long chain fatty acids such as carnauba wax, and ethylene bisstearin. Bisamide-based waxes such as acid amide are known, but all of these conventional 1m formulations satisfy all of the requirements of moisture resistance, reliability such as high-temperature electrical properties, releasability, and imprintability on the surface of molded products. It was nothing special.

In other words, long-chain fatty acids and their metal salts have good releasability and imprintability (
On the other hand, although it is relatively good, it has been recognized that failures tend to occur in reliability tests such as the pressure Kutsuker test and the pressure Kutsuker bias test, and that the moisture resistance is poor. In addition, although ester waxes have excellent base release properties and reliability, they are inferior in stamping properties, and especially as the number of molding cycles increases (: the stamping properties deteriorate extremely.) Bisamide waxes (4) Although it was excellent, it had the disadvantage of poor mold release properties.

[Purpose of the invention]

The present invention was made as a result of intensive studies to solve the above-mentioned drawbacks, and it involves adding a specific divalent fatty acid bisamide compound as an internal mold release agent to the conventional epoxy resin for encapsulating semiconductors (Secondly, An IC that has excellent reliability such as moisture resistance and high temperature electrical properties, and has good mold releasability.
ζ to provide a resin composition for semiconductor encapsulation that has good marking properties on a molded earthen product.

[Structure of the invention]

The present invention provides (1) a resin composition for semiconductor encapsulation, characterized in that it contains an epoxy resin and a divalent fatty acid bisamide compound represented by formula [A] in an amount of 0.01 to 10% by weight, CH , +OH, NHCO+CH, +mC0NH(-
(, 'H, +nCH, [A] (J, n is an integer of 14 or more, m is an integer of 3 or more) and (2) the divalent fatty acid bisamide compound is a divalent fatty acid with 5 or more carbon atoms and a divalent fatty acid with 15 or more carbon atoms. The resin composition for semiconductor encapsulation according to claim 1, characterized in that it is formed by condensing a long-chain aliphatic primary amine, and (3) the divalent fatty acid bisamide compound has a melting point of 80°C or more. 1
The resin composition for semiconductor encapsulation according to claim vX1, characterized in that the temperature is 40°C.

The present invention:: The epoxy resin used is bisphenol A
Type epoxy resin, Novo 2 Tsuku type epoxy resin, resorcinol epoxy resin, halogenated epoxy resin, glycidyl ester reduced epoxy resin, polymer type epoxy resin, etc., and the curing agent is monoamine type curing. agent, aliphatic polyamine, polyamide resin, aromatic diamine, acid anhydride curing agent Lewis acid complex compound, aromatic polyamine, polycarboxylic acid, polycarboxylic acid hydrazide, boron trifluoride monoethylamine, dicyandiamide, imidazole, phenolic resin , melamine resin, acrylic resin, area resin,
Isocyanate, etc., and fillers include glass fiber,
Metal Quisker, carbon fiber, Kepler fiber, polyester fiber, polyamide fiber, pulp, asbestos, crystalline silica, fused silica, alumina, calcium carbonate, magnesium carbonate, calcium hydroxide, aluminum hydroxide, antimony trioxide, Merck, titanium oxide etc. can be added. Other additives that can be added include coloring agents such as carbon black and iron oxide, and coupling agents. Also requires regular curing accelerator;
2. May be added accordingly.

The mold release agent used in the present invention, a divalent fatty acid bisamide compound, is represented by formula [A].

CH, (-CH, ÷, NHCO+CH,)-, C0N
H ÷ CH, ÷, CH.

(j and n are integers of 14 or more; m is an integer of 3 or more) In addition, it is also possible to use a conventionally commonly used mold release agent. The amount of the divalent fatty acid bisamide compound added is not particularly limited, but is preferably 0.01 to 10% by weight. That is, 0.01% divalent fatty acid bisoxide
Below 10%, the effect as a mold release agent is not expressed, and on the contrary,
This is because if it exceeds the epoxy resin, the crosslinking density after curing of the epoxy resin will drop significantly, and the mechanical properties, electrical properties, etc. of the cured product will be impaired, and the protective function of the semiconductor element will no longer be fulfilled.

Further, the divalent fatty bisamide compound represented by formula [A] can be obtained by condensing a divalent fatty acid having 5 or more carbon atoms with a long-chain aliphatic primary amine having 15 or more carbon atoms.

The present invention uses a divalent fatty acid bisamide compound represented by formula [A] as an internal mold release agent for epoxy resin (
The method of the present invention makes it possible to provide a resin composition for semiconductor encapsulation that satisfies all of the requirements such as reliability, releasability, and imprintability.

Conventional amide waxes have better heat resistance than other waxes, so they are widely used as internal mold release agents for molding materials. In other words, even if the molding process is repeated for a long time in a high-temperature mold, the wax that oozes out on the mold surface has good heat resistance. The reason for this is that it does not significantly damage the appearance of the product.However, while conventional amide waxes have excellent continuous moldability and are good in reliability and stampability, they have poor mold release properties. was insufficient.

Most conventional amide waxes are made by reacting intramolecular polyamide compounds obtained by condensing higher fatty acids such as stearic acid, behenic acid, or montanic acid with polyvalent amines such as ethylenediamine, or by reacting higher fatty acids with ammonia. (; It is an intramolecular polyamide compound that is methylolated and condensed with formalin, and has high polarity and is compatible with epoxy resins etc. (= other higher fatty acids, metal salts of higher fatty acids, higher fatty acids) Wax such as ester: Even if the same amount is added as an internal dispersing agent, the amount of wax that oozes out from the surface of the molded product and the mold surface will be extremely small, resulting in poor mold releasability. It will be done.

Further, such higher fatty acid intramolecular polyamide compounds have high crystallinity and a melting point as high as 115° C. to 160° C., which is also one of the reasons why the mold releasability is poor.

In addition to intramolecular polyamide compounds (higher fatty acid terminal amide compounds that are amidated by reacting secondary fatty acids with ammonia and unsaturated fatty acid intramolecular polyamide compounds), these have a relatively low melting point of 80 to 130℃. Although they are waxes, they all have poor heat resistance and are unsatisfactory in terms of long-term moldability.

Therefore, the inventors of the present invention made extensive studies to take advantage of the heat resistance, reliability, and good marking properties of amide waxes to further improve mold release properties. The divalent fatty acid bisamide compound obtained by condensing a saturated fatty acid with a long-chain aliphatic primary amine having 15 or more carbon atoms has a melting point of 80 to 140"C. The present invention was completed based on the knowledge that it has good moldability and also satisfies long-term moldability, reliability, and stamping properties.The number of carbon atoms in the divalent saturated fatty acid was reduced to 5 The reason why the number of carbon atoms in the long-chain aliphatic primary amine is specifically limited to 15 or more is that divalent fatty acid bisamide compounds obtained by condensing together those having less than this number of carbon atoms cannot exhibit mold release properties, and This is because if a divalent fatty acid having a number of 4 or less is used, the crystallinity will be high and the melting point will be 140°C or higher, which also causes a decrease in mold releasability.

〔Effect of the invention〕

The present invention is characterized in that an epoxy resin composition C consisting of an epoxy resin, a curing agent, a filler, and various additives is blended with a specific divalent fatty acid bisamide compound as an internal release agent. Suitable for molding a large number of electronic parts by molding, injection molding, etc.; satisfies reliability, stampability, mold releasability, and continuous moldability.

Next: The present invention will be explained in more detail by way of examples.

〔Example〕

In the following, parts refer to parts by weight unless otherwise specified.

Example 1゜Adipic acid (HOOC(-(,'H,+4COOH)
146 # (1 mol), stearylamine (C*5H
syN) 5381 (2-t=)v) and 100 LJ of toluene, thermometer, reflux condenser, IA equipped with a stirrer! Pour into a three-bottle flask and add 1 while stirring.
Heated until 20°C (120'C to 130°C)
The condensation reaction between carboxylic acid and amine becomes active, but the reaction system is maintained at 120-130''C for about 3 hours while the water produced is azeotropically removed with toluene and removed from the system.

Next: The temperature was gradually raised to 180° C. over 2 hours to complete the condensation reaction. Toluene remaining in the reaction system was removed under reduced pressure, and the product was taken out at a temperature of 130°C or higher and solidified by cooling.

The melting point of the reaction product was measured and found to be 136°C. On the other hand, when the infrared absorption spectrum of the product was measured, the carbonyl absorption of 1710 cIIL-1 of the raw material carboxylic acid disappeared beforehand, and instead, the carbonyl absorption of 1-niamide appeared at 1640α-1, indicating that it was a divalent carboxylic acid. It was confirmed that the amine condensation reaction occurred almost quantitatively, and the resulting reaction product was the desired divalent fatty acid bisamide compound.

Next, 5.5 parts of this divalent fatty acid bisamide compound was used as an internal dissipating agent, 100 parts of cresol novolac epoxy (M220 per epoxy), 30 parts of brominated phenol novolac epoxy (epoxy equivalent: 300), and a phenol novolac curing agent (molecular weight: 750). ) 60 parts, 0.5 parts of 2-ethyl-4-methylimidazole, 400 parts of crystalline silica powder, 2.0 parts of silane coupling agent, 30 parts of antimony trioxide, and 2.0 parts of carbon black; The molding material obtained by mixing and kneading was used as a resin composition for semiconductor encapsulation.

Example 2° Speric acid (H00C4-eH, +6eoOH) 174
N (1 mol), stearylamine 538! I (2 mol) and 130 toluene were reacted in the same manner as in Example 1 to obtain a divalent fatty acid bisamide compound. The melting point of this compound was 128°C. Subsequently, 35 parts of this compound was A mold release agent was blended in the same composition as in Example 1 to obtain a resin composition for semiconductor encapsulation.

Example 3 Sepacic acid (HOOC+CH,su,(,'0OH)
202.9 (1 mol), stearylamine 538 N
(2so/I/) and toluene 150= were reacted in the same manner as in Example 1 to obtain a higher fatty acid intramolecular monoamide compound. The melting point of this compound was 123°C. A resin composition for encapsulating a semiconductor was obtained by blending the same composition as in Example 1, using the following ingredients as an internal dissipating agent.

Example 4. .

An epoxy resin composition for semiconductors was obtained by blending 5.0 parts of the divalent fatty acid bisamide compound obtained in Example 1 and 0.5 parts of carnauba wax as an internal mold release agent in the same composition as in Example 1. Ta.

Comparative Examples 1 to 6 Six types of epoxy resin compositions for semiconductors were prepared using the same compositions as in Example 1 except for those listed in Table 1 below as an internal mold release agent.

Table 1 The above composition was molded using a transfer molding machine) at a pressure of 60 y.
Yyycu? A molded article was molded at a metal temperature of 175° C. for 2 minutes and 30 seconds, and further air-boosted at 175° C. for 4 hours to obtain a semiconductor sealed article. The mold releasability during molding, the long-term moldability, the reliability of the molded product, and the stampability were as shown in Table 2. Evaluation of each characteristic was performed as follows.

(a) Mold releasability Among the upper and lower molds, only the lower mold was equipped with a knock bottle, and continuous molding was carried out, and the molded product was easily attached to the upper mold (without knock bottle) and evaluated by the number of moldings at which it did not come loose.

(b) Long-term moldability The surface of the mold is in a mirror-like state (in two cases, continuous molding was performed and the surface of the molded product was dirty [appearance; indicated by the number of moldings when cloudiness began to occur).

(C) Reliability.

The resulting IC encapsulation was subjected to a pressure test (PC, 'T: 120° C. steam, 2 atm) to examine corrosion of the aluminum wiring. The occurrence of open circuits due to aluminum corrosion was detected and expressed as the initial failure occurrence time.

(d) Stamping property The surface of the IC package obtained was stamped with 97224 silver ink manufactured by Markem, and after ink air was applied at 150°C for 1 hour, a peeling test was performed with cellophane tape to ensure that even the slightest characters were missing. If there is, it is considered defective.

Table 2 ×...500 times or less 3 0...1200 hours or more, △...800~
1200 hours, ×... 800 hours or less

Claims (3)

[Claims] (1) A resin composition for semiconductor encapsulation, comprising an epoxy resin and a divalent fatty acid bisamide compound represented by formula [A] in an amount of 0.01 to 10% by weight. ▲There are mathematical formulas, chemical formulas, tables, etc.▼ (l, n are integers of 14 or more, m is an integer of 3 or more) (2) The divalent fatty acid bisamide compound is obtained by condensing a divalent fatty acid having 5 or more carbon atoms with a long-chain aliphatic primary amine having 15 or more carbon atoms. Resin composition for semiconductor encapsulation. (3) The melting point of the divalent fatty acid bisamide compound is 80 to 14
The resin composition for semiconductor encapsulation according to claim 1, characterized in that the temperature is 0°C.