KR20090119734A - Manufacturing method of resin composition for semiconductor element sealing - Google Patents

Abstract

The present invention provides the following components (A) to (C): (A) an epoxy resin; (B) curing agent; And (C) a method for producing a resin composition for sealing semiconductor elements comprising an inorganic filler, comprising (A) component and (B) component having an average particle diameter of 5 µm to 50 µm, further comprising (C) component Obtaining a mixture to make; Storing the mixture in a vessel for feeding the melt-kneader; Feeding the stored mixture from the vessel to a melt-kneader to obtain a kneading material; And a process of cooling and solidifying the kneaded material to be pulverized.

Resin composition for semiconductor element sealing, melt-kneading, segregation suppression

Description

Manufacturing method of resin composition for semiconductor element sealing {METHOD FOR PRODUCING RESIN COMPOSITION FOR SEMICONDUCTOR ELEMENT ENCAPSULATION}

This invention relates to the manufacturing method of the resin composition for semiconductor element sealing used in order to seal a semiconductor element.

Conventionally, semiconductor elements, such as a transistor, IC, and LSI, are sealed using the resin composition containing an epoxy resin, a hardening | curing agent, an inorganic filler, etc. In general, in the production of a resin composition for sealing a semiconductor device in solid state, a step is taken in which a blended component is mixed and melt-kneaded, followed by rolling and pulverizing a cooled solidified product (Japanese Patent Laid-Open No. 2007-77333, Japanese Patent). Japanese Patent Application Laid-Open No. 2006-297701 and Japanese Patent Laid-Open No. 2001-64398.

In the manufacturing process of the said resin composition, in order to raise manufacturing efficiency, the mixture of a compounding component is manufactured in advance in large quantities, and continuously melt-kneading, supplying to a melt-kneading machine is performed. For example, a melt-kneader 1 having a heater 3, a rotor blade 4, and a mixing chamber 5 shown in FIG. 1, and a container for supplying the mixture to the melt-kneader 1 ( When a melt-kneading apparatus including a hopper 2 (hereinafter referred to as a supply container) is used, a large amount of the mixture is temporarily stored in the hopper 2, and the melt-kneader 1 is removed from the hopper 2. The melt-kneading is performed continuously by supplying to the.

However, during the feeding of the mixture from the hopper 2 to the melt-kneader 1, a part of the compounding components segregates in the hopper 2, and as a result, of the resin composition obtained at the beginning and the end of the melt-kneading. Since the composition ratio slightly changed, there was a problem that the physical properties of the resin composition were changed. This is presumably because some of the compounding components stay on the wall surface of the hopper 2. For this reason, although there is a possibility that the shape of the hopper 2 can be improved by changing the shape of the hopper 2 conventionally used, changing the manufacturing conditions for each shape is a problem in terms of production efficiency. There is.

In addition, segregation of a part of the compounding components is not limited to the case of using a melt-kneading apparatus having a hopper as a supply container, but may also occur when melt-kneading using a ribbon mixer or the like as a supply container.

This invention is made | formed in view of such a situation, and in the manufacture of the resin composition for semiconductor element sealing provided with the process of supplying a mixture from a supply container, such as a hopper or a ribbon mixer, to a melt-kneading machine, and melt-kneading, The retention of components in the container can be prevented without affecting the shape or capacity of the supply container, and as a result, the variation of the composition ratio of the resin composition due to segregation of a part of the compounding component is suppressed, and the physical properties It aims at providing the manufacturing method of the stable resin composition for semiconductor element sealing.

Specifically, the present invention relates to the following items (1) to (3).

(1) This invention is (A) epoxy resin; (B) curing agent; And (C) a method for producing a resin composition for sealing semiconductor elements comprising an inorganic filler,

Obtaining a mixture containing component (A) and component (B) having an average particle diameter of 5 μm to 50 μm, further comprising component (C);

Storing the mixture in a vessel for feeding the melt-kneader;

Feeding the stored mixture from the vessel to a melt-kneader to obtain a kneading material; And

Cooling and solidifying the kneading material

The manufacturing method of the resin composition for semiconductor element sealing containing a.

(2) The average in which the spherical equivalent weight in the average particle diameter represented by following formula (1) of the said (A) component and (B) component is represented by following formula (1) of (C) component The manufacturing method of the said resin composition which is 0.4-20 times with respect to the spherical equivalent weight in particle diameter.

Spherical terms of the average particle diameter by weight d = [πd ^3/6 × (weight);

(Wherein d is an average particle diameter measured using a laser diffraction / scattering particle size distribution analyzer, and specific gravity is a value measured according to JIS-K6911)

(3) The manufacturing method of the said resin composition of (1) or (2) whose average particle diameters of the said (A) component and (B) component are 15-25 micrometers.

According to the present invention, when an epoxy resin (component A) and a curing agent (component B) adjusted to have an average particle diameter of 5 µm to 50 µm, an epoxy resin (component A), a curing agent (component B) and an inorganic filler (C When the mixture of components) is supplied from the supply vessel such as a hopper or a ribbon mixer to the melt-kneader, the retention of the compounding component in the supply vessel can be prevented without affecting the shape or capacity of the supply vessel. As a result, segregation of the said component can be suppressed and the resin composition for semiconductor element sealing with stable physical property can be obtained.

Next, embodiment of this invention is described in detail.

The resin composition for semiconductor element sealing manufactured by the manufacturing method of this invention contains the following (A)-(C) component.

(A) epoxy resin

(B) curing agent

(C) inorganic filler

In the manufacturing method of the resin composition for semiconductor element sealing of this invention, the epoxy resin (component A) and hardening | curing agent (component B) whose average particle diameters were adjusted to 5 micrometers-50 micrometers are used. The epoxy resin (component A) and hardening | curing agent (component B) adjusted to these predetermined average particle diameters may be grind | pulverized, and the commercial item adjusted so that it may become a predetermined average particle diameter may also be used.

When the average particle diameter of the epoxy resin (component A) and the curing agent (component B) exceeds 50 µm, a mixture of the epoxy resin (component A), curing agent (component B) and inorganic filler (component C) is melted from the supply container. When feeding to the kneader, some of the blending components may remain in the supply vessel. In particular, the content of the inorganic filler (component C) in the resin composition is increased in the late kneading. In addition, epoxy resins (component A) and curing agents (component B) having an average particle diameter of less than 5 µm are generally difficult to obtain and are not practical.

In order to suppress segregation of a component more effectively, it is preferable to use the epoxy resin (component A) and hardening | curing agent (component B) adjusted so that average particle diameter might be 15 micrometers-25 micrometers.

The average particle diameter of the epoxy resin (component A), the curing agent (component B) and the inorganic filler (component C) can be measured by analyzing a sample which is randomly extracted from the population of each component using a laser diffraction / scattering particle size distribution measuring device. Can be.

In this invention, the spherical equivalent weight in the average particle diameter represented by following formula (1) of A component and B component adjusted to the predetermined average particle diameter is in the average particle diameter represented by following formula (1) of C component. It is preferable that it is 0.4-20 times with respect to the spherical equivalent weight. If it exceeds 20 times, when the mixture of the epoxy resin (component A), curing agent (component B) and inorganic filler (component C) is continuously supplied from the supply vessel to the melt-kneader, the mixture remains in the supply vessel. Segregation of the above components can easily occur. In particular, there exists a tendency for content of the inorganic filler (C component) in the resin composition manufactured by the kneading | mixing late to become high. In addition, segregation of components tends to occur even if less than 0.4 times.

<Equation 1>

Spherical terms of the average particle diameter by weight d = [πd ^3/6 × (weight);

(Wherein d is an average particle diameter measured using a laser diffraction / scattering particle size distribution analyzer, and specific gravity is a value measured according to JIS-K6911)

In addition, when grind | pulverizing an epoxy resin (component A) and a hardening | curing agent (component B) so that it may become a predetermined | prescribed average particle diameter, a turbo mill etc. can be used as a grinder from a viewpoint of being easy to obtain a desired particle diameter efficiently. In this case, the epoxy resin (component A) and the curing agent (component B) may be separately ground so as to have an average particle diameter of 5 µm to 50 µm, and the epoxy resin (component A) and the curing agent (component B) are previously prescribed in a predetermined ratio. After mixing, it may be pulverized so that the average particle diameter is 5 μm to 50 μm. Moreover, after mixing an inorganic filler (component C) with an epoxy resin (component A) and a hardening | curing agent (component B) in predetermined ratio previously, it can also grind | pulverize so that an average particle diameter may be 5 micrometers-50 micrometers, but an epoxy resin (A It is preferable to grind before mixing with an inorganic filler (component C) from a viewpoint of being easy to confirm the average particle diameter and specific gravity of a component) and a hardening | curing agent (component B).

Moreover, in the manufacturing method of the resin composition for semiconductor element sealing of this invention, in addition to an epoxy resin (A component), a hardening | curing agent (B component), and an inorganic filler (component C), the hardening accelerator mentioned later, a flame retardant, pigments, including carbon black, etc. In addition, various additives to add as needed can be used.

These optical additives may be added when the epoxy resin (component A) and the curing agent (component B) are pulverized, and may be added during the mixing of the epoxy resin (component A), the curing agent (component B) and the inorganic filler (component C). It may be. Mixing can be performed as a mixer, for example using a Rodige mixer, Henschel mixer, etc.

Subsequently, a mixture of the epoxy resin (component A), the curing agent (component B), and the inorganic filler (component C) adjusted to a predetermined average particle diameter is added to the supply container and stored until melt-kneading.

The container for supply used by the manufacturing method of the resin composition for semiconductor element sealing of this invention is not restrict | limited, For example, the container which has a storage function and a supply function, such as a hopper and a ribbon mixer, can be used, and also depends on the capacity I never do that. Moreover, you may connect and use multiple supply containers. For example, a container such as one in which the outlet of the ribbon mixer is connected to the inlet of the hopper may also be used.

Then, the mixture is fed from the supply vessel to the melt-kneader according to the capacity of the melt-kneader and continuously melt-kneaded at 60 to 160 ° C. 1 shows a schematic configuration diagram of a melt-kneading apparatus used in the present invention. That is, in this melt-kneading apparatus, the hopper 2 is provided in the melt-kneader 1 as a supply container, and the melt-kneader 1 is provided with a heater 3 and a rotor blade 4. One mixing chamber 5 is installed. The mixture introduced into the hopper 2 is designed to be supplied from the hopper 2 to one end of the melt-kneader 1, and the mixture is discharged from the other end.

Finally, the obtained kneaded mixture is cooled and solidified and the solidified mixture is pulverized to 10 to 2000 µm, whereby a resin composition for semiconductor element sealing is obtained.

It does not specifically limit as an epoxy resin component (component A) used by the manufacturing method of the resin composition for semiconductor element sealing of this invention. For example, dicyclopentadiene type epoxy resin, cresol novolak type epoxy resin, phenol novolak type epoxy resin, bisphenol type epoxy resin, biphenyl type epoxy resin, tris (hydroxyphenyl) methane type epoxy resin, etc. Epoxy resins can be used. These epoxy resins may be used independently and may be used together 2 or more types. As the epoxy resin used in the present invention, the epoxy equivalent is 150 to 250, the softening point or the melting point is 50 to 130 ° C, and is solid at room temperature from the viewpoint of securing the suitable toughness after curing of the epoxy resin and the reactivity of the epoxy resin. Among them, in view of reliability, a cresol novolak type epoxy resin, a biphenyl type epoxy resin, or a moisture absorption type epoxy resin in which a lower alkyl group is added to the phenyl ring can be preferably used.

The curing agent (component B) is not particularly limited as long as it causes a curing reaction with an epoxy resin (component A), and examples thereof include acid anhydrides, phenol resins, amines, thiols, and the like. Among them, storage stability, curability, It is preferable to use a phenol resin from the point which is excellent in the physical property of a hardened | cured material. As a phenol resin, a dicyclopentadiene type phenol resin, a phenol novolak resin, a cresol novolak resin, a phenol aralkyl resin etc. are used, for example. These phenol resins may be used independently and may be used together 2 or more types. And as a phenol resin, it is preferable to use a hydroxyl equivalent of 70-250 and a softening point of 50-110 degreeC from a viewpoint of the reactivity with an epoxy resin (component A), and especially a phenol novolak resin from a viewpoint of high hardening reactivity. Can be preferably used. In addition, a low hygroscopic property such as a phenol aralkyl resin or a biphenyl aralkyl resin can be preferably used in view of reliability.

And the compounding ratio of an epoxy resin (component A) and a phenol resin (component B) is 0.5 degree with respect to 1 equivalent of epoxy groups in an epoxy resin (component A) from a viewpoint of hardening reactivity. The sum total of the hydroxyl groups in a phenol resin (component B) is 0.5. It is preferable to mix | blend so that it may be -2.0 equivalent, More preferably, it is 0.7-1.5 equivalent.

The inorganic filler (component C) is not particularly limited, and various conventionally known fillers can be used. For example, powder, such as quartz glass, talc, silica (fused silica, crystalline silica, etc.), alumina, aluminum nitride, and silicon nitride, is mentioned. These may be used independently and may be used together 2 or more types. Among them, silica powder is preferably used in view of the fact that the thermal linear expansion coefficient of the resulting cured product is reduced and internal stress can be reduced, so that warpage of the substrate and the element after resin sealing can be suppressed. It is more preferable to use powder in terms of high filling properties and high fluidity.

As an inorganic filler (component C), in order to prevent segregation of a compounding component more effectively, it is preferable to use the thing of the range of 0.5-45 micrometers, and it is more preferable to use the thing of the range of 5-35 micrometers.

It is preferable to set content of an inorganic filler (C component) in 50 to 90 weight% of the whole resin composition for semiconductor element sealing. Especially preferably, it is 60 to 90 weight%. That is, if it is less than 50 weight%, the linear expansion coefficient of hardened | cured material becomes large, the stress with respect to the semiconductor element to seal becomes large, and a function fall and the crack by temperature change become easy to occur. Moreover, when it exceeds 90 weight%, it is because the tendency for the viscosity of an epoxy resin composition to become high and moldability will fall is seen.

Moreover, in the manufacturing method of the resin composition for semiconductor element sealing of this invention, in addition to an epoxy resin (component A), a hardening | curing agent (component B), and an inorganic filler (component C), as mentioned above, a hardening accelerator, a flame retardant, and a mold release agent as needed. And other additives such as pigments including carbon black can be appropriately blended.

As a hardening accelerator used by this invention, if it accelerates hardening reaction of an epoxy resin (component A) and a hardening | curing agent (component B), it will not specifically limit, Conventionally well-known various hardening accelerator can be used. For example, a phosphorus hardening accelerator, an amine hardening accelerator, a diazabicyclo alkene hardening accelerator, etc. are mentioned.

As a flame retardant, organophosphorus compound, antimony oxide, metal hydroxides, such as aluminum hydroxide and magnesium hydroxide, etc. are mentioned, for example. These may be used alone or in combination of two or more thereof.

The sealing method of the semiconductor element using the resin composition for semiconductor element sealing obtained by the manufacturing method of this invention is not specifically limited, It can carry out by well-known shaping | molding methods, such as a transfer molding method. In addition, the resin composition for semiconductor element sealing can also be used in powder form as it is, and can also be used by shape | molding in tablet form.

<Example>

Next, an Example is demonstrated with a comparative example. However, the present invention is not limited to these examples.

First, each component shown below was prepared.

Epoxy resin a: Biphenyl type epoxy resin (Epoxy equivalent: 190, Melting point: 105 degreeC, Specific gravity: 1.2)

Epoxy resin b: Cresol novolak-type epoxy resin (epoxy equivalent: 195, softening point: 75 degreeC, specific gravity: 1.2)

Curing agent: Phenolic novolac resin (hydroxyl equivalent: 110, softening point: 100 ° C, specific gravity: 1.2)

Inorganic filler a: Crushed fused silica powder with an average particle diameter of 8 μm and a specific gravity of 2.2

Inorganic filler b: spherical fused silica powder with an average particle diameter of 30 μm and a specific gravity of 2.2

Inorganic filler c: Crushed fused silica powder with an average particle diameter of 15 μm and a specific gravity of 2.2

Curing Accelerator: Triphenylphosphine

Release Agent: Carnauba Wax

Silane coupling agent: γ-glycidoxypropyltrimethoxysilane

Pigment: Carbon Black

Flame Retardant: Antimony Trioxide

Examples 1-4, Comparative Examples 1-4

Table 1 shows the compositions of the resin compositions I and II for sealing semiconductor elements prepared in Examples 1 to 4 and Comparative Examples 1 to 4. After mixing an epoxy resin (component A) and a hardening | curing agent (component B) in the composition shown in Table 1, Examples 1-4 were turbo mill and Comparative Examples 1-4 were changed suitably as a grinder, and conditions were changed suitably. By pulverizing, the resin compound of the epoxy resin (component A) and hardening | curing agent (component B) which have the average particle diameter shown in Table 2 and Table 3 was obtained.

Then, the resin blend, the inorganic filler (component C), and the other additives shown in Table 1 were dispersed for 2 minutes using a Henschel mixer (capacity: 200 L) as a mixer so that the total amount of all components became 100 kg at the ratio shown in Table 1. The mixture was obtained by mixing.

In addition, the average particle diameter of a resin compound and an inorganic filler (component C) is computed by measuring the particle size distribution of each component by the wet method using the laser diffraction / scattering particle size distribution analyzer LA-910 by HORIBA, Ltd. It was.

The mixture was then introduced into a hopper (volume: 400 L), which was a supply vessel provided in the melt-kneading apparatus. This process was repeated twice to make the mixture in the hopper total 200 kg.

The mixture in the hopper was melt-kneaded (temperature: 80 ° C.) while continuously feeding the screw-type melt-kneader from the hopper at a flow rate of 200 kg / hour. The kneading mixture discharged from the screw-type melt-kneader was taken six times at three minute intervals from the start of the discharge, followed by one time after 20 minutes, and seven times at three minute intervals. Each kneaded mixture taken at each time was rolled with a calender roll to air-cool and solidified, and each kneaded mixture obtained by air-cooled was pulverized using a hammer-type grinder to obtain 14 of each resin composition in Examples 1-4 and Comparative Examples 1-4. Samples were obtained.

Resin composition evaluation method 1

Transfer molding of a tablet having a diameter of 30 mm from the 14 samples (30 g) of each of the resin compositions in Examples 1 to 4 and Comparative Examples 1 to 4 obtained by the above method and preliminary heating to 80 ° C. : 175 degreeC x 2 minutes), After performing the post hardening of 175 degreeC x 5 minutes, the test piece for specific gravity measurement was obtained, and specific gravity was measured. And the fluctuation range of specific gravity was computed in 14 samples of each resin composition in Examples 1-4 and Comparative Examples 1-4. The variation range of the specific gravity means the difference between the maximum value and the minimum value in 14 samples. In addition, the specific gravity measurement method was based on JIS-K6911.

Resin composition evaluation method 2

Moreover, using 14 samples of each resin composition obtained by the said method, the spiral flow measurement in 175 degreeC was performed according to ASTMD3123-98 (2004). And the fluctuation range of the spiral flow length was computed in 14 samples of each resin composition in Examples 1-4 and Comparative Examples 1-4. The fluctuation range of the helical flow length means the difference between the maximum value and the minimum value in 14 samples.

As a result, as shown in Table 2 and Table 3, the sample of the Example whose average particle diameter of the resin compound is 5 micrometers-50 micrometers compared with the sample of the comparative example whose average particle diameter of the resin compound exceeded 50 micrometers, Fluctuations in specific gravity and spiral flow length were suppressed. That is, in the manufacturing method of the resin composition for semiconductor element sealing of this invention, when the resin mixture is continuously melt-kneaded, the change of the physical property of a resin composition is small and stable manufacture can be performed in the early stage of melt-kneading and a late stage.

While the present invention has been described in detail and specific embodiments thereof, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

This application is based on Japanese Patent Application No. 2008-128035, filed on May 15, 2008, the entirety of which is incorporated herein by reference.

The references cited herein are also incorporated by reference in their entirety.

BRIEF DESCRIPTION OF THE DRAWINGS It is a block diagram of the melt-kneading apparatus used preferably for the manufacturing method of the resin composition for semiconductor element sealing of this invention.

<Brief description of symbols for the main parts of the drawings>

1 melt-kneader

2 hopper

3 heater

4 rotor blades

5 mixing chamber

Claims (3)

(A) an epoxy resin; (B) curing agent; And (C) a method for producing a resin composition for sealing semiconductor elements comprising an inorganic filler, Obtaining a mixture containing component (A) and component (B) having an average particle diameter of 5 μm to 50 μm, further comprising component (C); Storing the mixture in a vessel for feeding the melt-kneader; Feeding the stored mixture from the vessel to a melt-kneader to obtain a kneading material; And Cooling and solidifying the kneaded material The manufacturing method of the resin composition for semiconductor element sealing containing a. The average particle diameter of the spherical equivalent weight in the average particle diameter represented by following formula (1) of the said (A) component and (B) component in the average particle diameter represented by following formula (1) of (C) component The manufacturing method of the resin composition for semiconductor element sealing which is 0.4-20 times with respect to the spherical equivalent weight of the. <Equation 1> Spherical terms of the average particle diameter by weight d = [πd ^3/6 × (weight); (Wherein d is an average particle diameter measured using a laser diffraction / scattering particle size distribution analyzer, and specific gravity is a value measured according to JIS-K6911) The manufacturing method of the resin composition for semiconductor element sealing of Claim 1 whose average particle diameters of the said (A) component and (B) component are 15-25 micrometers.

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