JPS5834824A - Epoxy resin composition and its production - Google Patents

Abstract

PURPOSE:To obtain an epoxy resin composition for semiconductor sealing having excellent moisture resistance and a low a stress, by adding strongly water-repellent flexible silane compound containing a silane coupling agent having a silanol functionality <=2 to a resin material and reacting the mixture under an alkaline condition or in contact with superheated steam. CONSTITUTION:A silane coupling agent, silane functionality <=2, and 0.5-3% silicone oil are premixed with part or the whole of at least one material containing a filler in contact with superheated steam or under an alkaline condition of pH>8. Then the mixture is mixed with the remaining portion of the material. The epoxy resin thus produced is mixed with a curing agent, a cure accelerator, a filler, a mold release, a surface-treating agent, etc., to obtain the title epoxy resin composition. This composition is excellent in moisture resistance, useful as a semiconductor-sealing resin having a low stress and particularly useful in the mass production of parts of electrical devices and instruments.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an epoxy resin composition for semiconductor encapsulation that has excellent moisture resistance and low stress, and a method for producing the same.
The characteristic line of the present invention is the addition of a flexible silanized compound with strong water transportability containing a silane coupling agent having a silanol functional group number of 2 or less, and the addition of a flexible silanized compound with strong water carrying properties, and the addition of a silanized compound under superheated steam aeration or dl? H)g〃The reaction is carried out under alkaline conditions.

The electronic equipment industry in Tokyo is rapidly developing, and numerous technological improvements are being made to maintain the characteristics of semiconductors.

Along with this, the rent for epoxy resin molding for semiconductor encapsulation has also increased.
In order to maintain the characteristics of semiconductors, the utmost care has been taken to maintain the properties of semiconductors. Among these requests, 41 is heavy! In other words, the stress transmission and temperature resistance of the epoxy sealing method are $4 or higher.In other words, stress such as strain generated during the hardening of the resin during the heat change during semiconductor assembly. The demand for the development of epoxy resin molding materials that are less susceptible to corrosion, such as small particles (and pellets generated due to water penetration), is increasing year by year. Typically,
The main cause of q# failure of semiconductors was the stress generated during thermal stress during the semiconductor assembly process when the sealing resin sludges, and the insulation with corrosion due to water intrusion. It was damaged by a short circuit in the destroyer circuit. In order to reduce the 41iF breakdown of these semiconductors, it is necessary to reduce the stress of the semiconductor sealing resin and to increase its moisture resistance.

Resin composition of the present inventors 0dPKIi Aqueous strong PKI II
It has been found that these technical problems can be solved by adding an ionic compound. That is, it has been discovered that the flexible Schiff-formed metal material prevents water from entering and serves as a stress buffer layer.

The present invention uses a silane coupling agent having a silanol functional group number of 2 or less and a silicone oil or a silicone rubber at 0.0%.
Epoxy resin compositions containing 6 to 396% mold, curing agents, curing accelerators, fillers, mold release agents, surface treatment agents, etc., and silane coupling agents with a silanol functional group number of 2 or less and 0.5 to 3% of silicone oil or silicone rubber, part or all of one or more raw materials containing fillers, and superheated steam aeration once aP!
Pre-mix under 80% condition, and then mix and knead with the remaining raw materials. A method for producing a resin composition is provided.

In order to achieve both am resistance and low stress, the silanol group must be
It is necessary to use a part of the silane coupling agent silicone oil or silicone rubber.

If the number of silanol groups is 3 or more, the crosslinking density will not be high and the flexibility will be lost, so the number of silanol groups in the silane coupling agent must be 2 or less. Furthermore, the stress reduction is insufficient with the length of the silane coupling agent, and the length of the silicone oil or silicone rubber cannot make fillers such as silica powder hydrophobic, that is, the moisture resistance is poor. It is necessary to use them together. In particular, it is desirable that the silane coupling agent silicone oil or silicone rubber used has a functional group (for example, an aino group, an alkyl group, an epoxy group, or a carboxyl group) that reacts with the epoxy resin medium curing agent. . Moreover, it is necessary to use 0.5 to 396 in quantity. This is because if it is less than OJ-, the effect of reducing stress will be small, and if it is more than 300, there will be harms such as a decrease in the glass transition point of the product and poor stamping properties.In addition, these silane coupling agents In order for silicone oil or silicone rubber to work effectively, it must be premixed with part or all of one or more raw materials containing fillers under superheated steam aeration or under conditions of pm>6.
It is necessary to mix and knead with the raw materials of IIK Residue.

In order to fully and uniformly bring out the moisture resistance and flexibility properties 2, it is important to mix well with the filler and to homogeneously disperse this mixture in the other raw materials. In addition, in order to completely carry out the hydrophobization reaction of the filler with the silane coupling agent, it is necessary to treat the filler and the silane coupling agent under superheated steam aeration and at a pH of 5%. Any other method will result in insufficient hydrophobization reaction and a decrease in temperature resistance. In addition, as a basic substance for adjusting pH)g, organic substances (for example, 2.L 4- L 7-8* 9*
10-Ootakydro-pyramido
(1,2-IL)&Je)in@group) is more desirable.

The present invention provides an epoxy resin composition for encapsulating semiconductors that is moisture resistant and has low stress due to humidity and a method for manufacturing the same, which is extremely useful industrially as it enables the large capacity of electronic components. Examples and comparative examples will be described below.

Example-1 Silica powder 67, 0.4 parts of a silane coupling agent with three silanol groups, 1 part of silane coupling agent 8-dalisidoxymethyldimethoxysilane with two silanol groups, and 0.5 parts of amino-modified silicone oil and 1.5-di! Zabishita stomach (4 u3t
O)/*y-5111 water $1 liquid (PIE>8) 0.1
1S & Mixed with Henschel (Kisa-) while spraying.Furthermore, 20 parts of epoxy resin, 10 parts of curing agent, 0.5 parts of curing accelerator, and 0.5 parts of lid release agent O3S were added and mixed. The stress (hereinafter referred to as stress) due to the semiconductor product O piezoresistor aK using this composition was -700 kF/-bending elasticity of the car horn 10,001 gF/
- So-called! pressure! Reliability test (PC?
) was 1400 hr (this is the conventional O level) stress was about half, and reliability was about 3 times higher. Semiconductor parts sealed with this composition from o-voo°C to 240°C
The results of the O temperature Nykle test (hereinafter referred to as TeC!) showed that the defective rate was about V6 compared to the conventional test.

Example-2 67 parts of silica powder, 0.5 parts of a conventional alicyclic epoxysilane coupling agent having 3 silanol groups, 271 parts of C-adenoglobil methyldiethoxy having 2 silanol groups, and silica; 2 parts of rubber was sprinkled on the mixture, and 7 o'clock steam was further injected six times at a rate of 5 seconds every 30 seconds to mix the mixture in a Ni-Goo. Furthermore, epoxy resin 208i! 1 part layering agent O, part OJ part SSa conversion agent added and mixed at 100C.
An epoxy resin composition was obtained by kneading it in an O-heated quart. The stress of a semiconductor product manufactured using this composition was 16001q/--
The elastic modulus is 900kt/ajPcT1300hr)
Ta.

Comparative Example-1 (-dashicytoxy, metherdimethodisilane, anno-modified silicone oil, and 1.5 cyanazyl
s (4s 3t O) , /$Bon-51t water-soluble at-tt The stress of the semiconductor product manufactured in the same manner as in Example-1 and sealed with a normal epoxy resin was 1,700 kf/csi. - The elastic modulus is 1600kf
/7pcT is 600 hr and 9.

Comparative Example-8 66 parts of silica powder, 0.5s of a silane coupling agent with three silanol groups, and a coupling agent with two silanol groups (-Mercapdobuvir, Methyldimethoxysilane 2)
1 part and 1.5 parts of epoxy-modified silicone oil (total 3 parts)
．． 5 parts) and 2-8# 416e 7*L
9e 10-octahydro-pimid-(1,2-
& ”) Add and mix 0.1 part of azepine 1-aqueous solution (pm) 8), then add 20 parts of epoxy resin, 10 parts of curing agent, 0.5 parts of lid release agent, O1S part, and curing accelerator = Knead with a kneader to obtain epoxy resin composition Using this composition, the stress and CT41 properties of nine semiconductor products were determined by Example Oka et al., and the glass transition point was as low as 132°C (TCT was poor and round).

The above results are summarized as follows: 011 It can be seen that when the poxy resin composition according to the present invention is used, the stress of semiconductor products is reduced and the moisture resistance is improved. It has been found that it has the following characteristics and is extremely useful industrially.

Claims (1)

[Claims] (1) A silane coupling agent having a silanol functional group number of 2 or less and silicone oil or silicone rubber at 0°8
-~3- An epoxy resin characterized by containing a curing agent,
Epoxy resin compositions that are effective as curing accelerators, fillers, mold release agents, surface treatment agents, etc. (Odor: Silane coupling agent with silanol functional groups of 2 or less;
- is premixed with part or all of one or more raw materials containing fillers under superheated steam aeration or under conditions of PH), and then mixed with the remaining raw materials and a human being mixed with A method for producing an epoxy resin composition comprising an epoxy resin as tatami mold, a curing agent, a curing accelerator, a filler, a mold release agent, a surface treatment agent, etc.