JP2002146233A - Surface-treated fine spherical silica powder and resin composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prepare fine spherical silica powder which can give a resin composition which, even when highly loaded with a filler, has a greatly improved fluidity and gives a molded article greatly improved in reliability without detriment to the dispersibility of the filler; and to obtain an inorganic filler and a resin composition, both prepared by using the same. SOLUTION: This fine spherical silica powder is surface-treated with a silane coupling agent and has an average particle size of 1.0 μm or lower and an average spheroidicity of 0.85 or higher. The silane coupling agent is used in an amount equivalent to 30-70% of all the specific surface area of the silica powder and has a carbon content of 0.05-5%. The silica powder is produced by spraying the silane coupling agent on raw fine spherical silica powder having an average particle size of 1.0 μm or lower and an average spheroidicity of 0.85 or higher and dispersed by a vibration fluidized bed. An inorganic filler and a resin composition, both containing the silica powder, are provided.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a solid or liquid resin used for semiconductor encapsulation and a resin substrate, which is excellent in dispersibility and filling property, and has improved heat resistance reliability and fluidity. And a resin composition using the same.

[0002]

2. Description of the Related Art Conventionally, in a semiconductor resin encapsulant, crystalline or amorphous silica spherical silica powder is crushed into solid or liquid resin for the purpose of reducing the coefficient of thermal expansion and improving heat resistance. Used in combination with silica powder or alone. For example, JP-A-2-173155 discloses that a spherical silica powder having an average particle diameter of 40 μm or less is used in combination with a crushed silica powder having an average particle diameter of 12 μm or less. Discloses that spherical silica powder is used alone.

[0003] However, if the ratio of silica powder in the resin composition is significantly increased, voids in the resin are hardly removed, resulting in a decrease in mechanical strength after molding and a decrease in fluidity during molding, thereby increasing productivity. Gets worse. In addition, in semiconductor encapsulation, there is a problem that various molding defects are likely to occur, such as deformation of a die on which a chip is mounted, flow or cutting of a gold wire.

Therefore, as a technique for preventing the moldability (fluidity) at the time of sealing the high filling area of the silica powder from being impaired, for example, a method of widening the particle size distribution (Japanese Patent Application Laid-Open No. Hei 6-80863) and a method of sphericity are disclosed. Higher method (JP-A-3-66151)
JP-A-5-2393), and a method of adding a small amount of a spherical fine powder having an average particle diameter of about 0.1 to 1.0 μm.
No. 21) has been proposed.

[0005] Among them, the method of adding a small amount of spherical fine powder is an effective method because the flow characteristics and burr characteristics of the sealing material are remarkably improved even in a high filling region of silica powder. Spherical fine powder tends to agglomerate and has a problem in dispersibility in a resin, so that in the high filling region of silica powder, today's further requirements cannot be sufficiently satisfied.

As a method of improving the fluidity by reducing the agglomeration of the spherical fine powder, a surface treatment is carried out with a different silane coupling agent such that the respective surfaces of the large particle powder and the fine powder are charged in the positive and negative directions. Method of attaching fine powder to the surface of large particle powder by electrostatic attraction (JP-A-5-3286)
No. 7), and among silica powders, a method has been proposed in which only large particle powders are subjected to silane coupling treatment, and fine powders that cause agglomeration are untreated and mixed to reduce aggregation. Japanese Patent Application Laid-Open No. Hei 8-20673).

However, these methods require that the surface treatment of the large particle powder is indispensable, and that each powder is charged in the opposite direction, so that the combination of silane coupling agents to be used is limited, Since the fine powder occupying most of the specific surface area has not been subjected to the silane coupling agent treatment, such a method has limitations in terms of improving strength and heat resistance reliability.

[0008]

SUMMARY OF THE INVENTION The present invention has been made in view of the above, and an object of the present invention is to provide an ultrafine spherical silica having an average particle size of 1.0 μm or less and an average sphericity of 0.85 or more. By treating the powder with a specific amount of a silane coupling agent, it is possible to suppress a decrease in the sphericity of the treated product, and as a result, it can be used alone or in combination with the base inorganic powder to form a solid or liquid resin. Fine spherical silica powder that can significantly improve the heat resistance of semiconductor resin encapsulants, etc. It is to provide a composition.

An object of the present invention is to disperse an average particle diameter of 1.0 μm or less and an average sphericity of 0.8
It can be achieved by spraying a predetermined amount of a silane coupling agent onto five or more fine spherical silica powders.

[0010]

That is, the present invention provides a silica powder having an average particle diameter of 1.0 μm or less and an average sphericity of 0.85 or more, which is surface-treated with a silane coupling agent. The fine spherical silica powder is characterized in that the amount of the agent is equivalent to 30 to 70% of the specific surface area of the raw silica powder and the carbon content is 0.05 to 5% (mass%, the same applies hereinafter). The silane coupling agent preferably has three alkoxy groups, and more preferably has 1 to 10 carbon atoms in the organic functional group directly bonded to Si.

In the present invention, the average particle diameter dispersed by the vibrating fluidized bed is 1.0 μm or less and the average sphericity is 0.8 μm.
A method for producing the above-mentioned fine spherical silica powder, which comprises spraying a silane coupling agent onto five or more fine spherical silica powder raw materials.

Further, the present invention is an inorganic filler characterized by containing the fine spherical silica powder in an amount of 3 to 30%.

Further, the present invention is a resin composition containing the above-mentioned fine spherical silica powder in an amount of 10 to 40%, and containing the above-mentioned inorganic filler in an amount of 70 to 95%. It is a resin composition.

[0014]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail.

The silane coupling agent used in the present invention includes vinyltrichlorosilane, vinyltriethoxysilane, vinyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, β (3,4 epoxy synchrohexyl) ethyltrisilane. Methoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropylmethyldiethoxysilane, N-β (aminoethyl) γ-aminopropyltrimethoxysilane, N-
β (aminoethyl) γ-aminopropylmethyldimethoxysilane, γ-aminopropyltriethoxysilane, N
-Phenyl-γ-aminopropyltrimethoxysilane,
γ-mercaptopropyltrimethoxysilane, γ-chloropropyltrimethoxysilane and the like can be used.

Of these, those having three alkoxy groups and the organic functional group directly bonded to Si having 1 to 10 carbon atoms are preferred. Specific examples thereof include γ-glycidoxypropyltrimethoxysilane,
γ-aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane.

Further, the fine spherical silica powder raw material to be surface-treated has an average particle diameter of 1.0 μm or less and an average sphericity of 0.85 or more, particularly 0.90 or more. 40 m ² / g, surface silanol group concentration is what is preferably 0.5 to 5.0 pieces / nm ^2. The average particle size is less than 0.10 μm and the specific surface area is 40 m ² /
When the average particle diameter exceeds 1.0 μm and the specific surface area is less than 5 m ² / g, the effect of improving the fluidity of the sealing material in the high filling region of the filler becomes insufficient.
On the other hand, the concentration of the silanol group was 0.5 / nm ²
In the case where the surface treatment is carried out with a silane coupling agent, the number of active sites where the silane coupling agent reacts is reduced, and the effect of reinforcing the strength of the semiconductor resin sealing material becomes insufficient. If the number exceeds 5.0 particles / nm ² , aggregation before the surface treatment is performed is large, and the amount of aggregation cannot be reduced even if the surface treatment is performed by performing the crushing treatment. Instead, the fluidity is reduced.

The amount of the silane coupling agent is an amount capable of treating 30 to 70% of the specific surface area of the fine spherical silica powder. If the amount is smaller than this, sufficient heat resistance and strength cannot be obtained, and if it exceeds 70%, the amount of aggregation increases, and a sufficient fluidity improving effect cannot be obtained.

In the present invention, the required amount of the silane coupling agent, that is, 30% of the specific surface area of the raw silica powder
The amount equivalent to ~ 70% can be determined by the following equation. Amount (g) of silane coupling agent = [{amount of raw silica powder (g) × specific surface area (m ² / g) × processing amount (g)} / minimum coverage area of silane coupling agent (m ² / g) )

Here, the minimum covering area of each silane coupling agent can be calculated as follows. That is, when the functional group is trialkoxysilane, Si (O) ₃ obtained by hydrolysis is converted into one spherical Si atom with a radius of 2.10 ° and three O atoms with a spherical shape with a radius of 1.52 °, and Si -O bond length 1.51 °, tetrahedral angle 10
Assuming 9.5 °, and further assuming that all three O atoms in the model react with the silanol groups on the silica surface, the smallest circular area that can be covered by the three O atoms is calculated. As a result, the coverage area per molecule was 1.33 × 1
0 ^-19 m ² / molecule, converted to 8.0 per mole
It becomes 1 × 10 ⁴ m ² / mol. The minimum coating area of each coupling agent can be determined by multiplying the minimum coating area value per mole by the molecular weight of each silane coupling agent. For example, in the case of γ-glycidoxypropyltrimethoxysilane having a molecular weight of 236.3, the minimum covering area is 330 m ² / g, and when the specific surface area of the raw silica powder is 20 m ² / g, the equivalent amount of 30 to 70% is as follows. And 1.8 to 4.2 g per 100 g of raw silica powder.

The determination as to whether or not the silica is actually treated with the optimum amount of the silane coupling agent is performed by measuring the carbon content of the silica surface after the treatment. As a specific method, a solvent capable of dissolving the silane coupling agent, for example, acetone, is washed several times to remove the unreacted silane coupling agent, and then dried, and then subjected to a carbon / sulfur simultaneous analyzer (eg, LECO).
Company, CS-444LS type).
The amount of the silane coupling agent bound to the fine spherical silica surface is calculated. In the present invention, the carbon content needs to be 0.05 to 5% in order to achieve the initial purpose.

In the surface-treated fine spherical silica powder of the present invention, the average particle diameter is specified to be 1.0 μm or less, and the average sphericity is specified to be 0.85 or more. This means that the average sphericity of the raw material silica powder has not deteriorated even if it was performed. The cause of the decrease in the average sphericity is considered to be the destruction of spherical silica due to shearing force during processing and the increase in aggregation due to the presence of the silane coupling agent. It is not preferable because it causes a decrease in fluidity and a decrease in fluidity.

The fine spherical silica powder of the present invention is prepared by adding a silane coupling agent to a raw material of fine spherical silica powder having an average particle diameter of 1.0 μm or less and an average sphericity of 0.85 or more dispersed in a vibration fluidized bed. It can be manufactured by spraying a fixed amount. Hereinafter, this will be described in more detail.

In the surface treatment of fine powder having an average particle size of 1.0 μm or less, dispersion due to excessive mechanical shearing force rather increases coagulation. Therefore, air, N ₂ gas or the like is placed under the porous dispersion plate from below. Is effective to suspend the powder on the dispersing plate and to make the powder fluidized by applying vibration, followed by surface treatment by adding a silane coupling agent. At this time, the addition of the silane coupling agent is desirably performed by spraying with a two-fluid nozzle or the like so that the droplet diameter is reduced as much as possible. The form of the silane coupling agent may be a stock solution, an aqueous solution, or an alcohol solution, or may be in a gaseous state vaporized to such an extent that the silane coupling agent is not decomposed. Further, a silane coupling agent, other spraying from above the vibration flow devices can be added and mixed air blown from below the dispersion plate, the N ₂ gas or the like.

As a guide of the processing conditions in the oscillating fluidized bed,
The amount of the silane coupling agent is adjusted so that the sphericity of the spherical silica powder decreases 10% or less (including 0), preferably 8% or less (including 0) due to the increase in aggregation by the silane coupling agent.・ Adjust seeds. If the degree of decrease in sphericity exceeds 10%, the fluidity and high packing property, which are advantages of spherical silica, are impaired, which is not preferable.

Further, by raising the temperature in the system and increasing the surface treatment temperature, it is possible to shorten the reaction time and suppress the change with time. The temperature in the system is within a temperature range in which the silane coupling agent does not thermally decompose. For example, when the silane coupling agent is γ-glycidoxypropyltrimethoxysilane, the temperature in the system is 20 to 1
The temperature is 80 ° C, preferably 80 to 150 ° C. As a method for increasing the temperature in the system, a general method such as a heating device or a heating jacket can be used, or heated air, N ₂ gas or the like can be blown.

The inorganic filler of the present invention comprises the fine spherical silica powder of the present invention and a base inorganic powder, and the total content of the fine spherical silica powder of the present invention is 3 to 30%.
It is composed of As the base inorganic powder, crystalline silica, amorphous silica, alumina, silicon nitride, aluminum nitride and the like are used, and the shape is spherical, crushed, square, or a mixture of two or more of these. Is also good. When the content of the fine spherical silica powder of the present invention is less than 3%, the effect of improving the fluidity of the resin composition is insufficient, and
%, The fluidity decreases due to an increase in viscosity.

When the application of the inorganic filler of the present invention is a sealing material, spherical amorphous silica, which can meet required properties such as low thermal expansion property and moisture resistance, is particularly preferable as the base inorganic powder. Among them, a base inorganic powder having a sphericity of 0.80 or more in a coarse powder region of 30 to 50 μm and a ratio of 30 to 50% in a fine powder region of 3 to 10 μm is preferable. On the other hand, in the case of a resin composition requiring high thermal conductivity, alumina, silicon nitride, aluminum nitride, or the like having high thermal conductivity is preferable.

The resin composition of the present invention filled with 10 to 40% of the fine spherical silica of the present invention is suitable for a resin substrate. If the filling amount is less than 10%, the required resin reinforcing effect cannot be obtained. On the other hand, if it is more than 40%, moldability and mechanical strength decrease due to an increase in resin viscosity and generation of voids.

Further, the inorganic filler of the present invention has a content of 70 to 95.
% Is particularly suitable as a resin composition for semiconductor encapsulation. When the filling amount is less than 70%, the resin reinforcing effect is insufficient. On the other hand, if it exceeds 95%, it is difficult to maintain good fluidity, and moldability deteriorates.

The resins used in the present invention include epoxy resins, silicone resins, phenol resins, melamine resins, urea resins, unsaturated polyesters, fluororesins, polyamides such as polyimide, polyamideimide and polyetherimide, and polybutylene terephthalate. , Polyester such as polyethylene terephthalate, polyphenylene sulfide, wholly aromatic polyester, polysulfone, liquid crystal polymer, polyether sulfone, polycarbonate,
Maleimide-modified resin, ABS resin, AAS (acrylonitrile-acrylic rubber-styrene) resin, AES (acrylonitrile-ethylene-propylene-diene rubber-styrene) resin and the like can be mentioned.

Among these, as the resin for semiconductor encapsulation,
An epoxy resin having two or more epoxy groups in one molecule, specifically, phenol novolak type epoxy resin, orthocresol novolak type epoxy resin, epoxidized novolak resin of phenols and aldehydes, bisphenol Glycidyl ethers such as A type, bisphenol F type and bisphenol S type, and glycidyl ester acid epoxy resins, linear aliphatic epoxy resins, and fatty acids obtained by reacting epochlorohydrin with polybasic acids such as phthalic acid and dimer acid Cyclic epoxy resin, heterocyclic epoxy resin, alkyl-modified polycyclic epoxy resin, β-naphthol novolak type epoxy resin, 1,6-dihydroxynaphthalene type epoxy resin,
2,7-hydroxynaphthalene type epoxy resin, bishydroxybiphenyl type epoxy resin and the like. Among them,
From the viewpoint of moisture resistance and solder reflow resistance, ortho-cresol novolak type epoxy resin, bishydroxybiphenyl type epoxy resin, and epoxy resin having a naphthalene skeleton are preferable. For the resin substrate, a glycidyl ether such as a bisphenol A type or a bisphenol F type having a low viscosity in a liquid state among the above epoxy resins is used.

The curing agent for the epoxy resin is not particularly limited as long as it reacts with the epoxy resin and cures. For example, phenol, cresol, xylenol,
Resorcinol, chlorophenol, t-butylphenol, nonylphenol, isopropylphenol, octylphenol and the like, formaldehyde, paraformaldehyde or a novolak resin obtained by reacting a mixture of two or more thereof together with paraxylene under an oxidation catalyst; Polyparahydroxystyrene resin, bisphenol compounds such as bisphenol A and bisphenol S, trifunctional phenols such as pyrogallol and phloroglucinol, maleic anhydride, acid anhydrides such as phthalic anhydride and pyromellitic anhydride, metaphenylenediamine, Examples thereof include aromatic amines such as diaminodiphenylmethane and diaminodiphenylsulfone.
Further, a curing accelerator can be blended to promote the reaction between the epoxy resin and the curing agent. Examples of the curing accelerator include 1,8-diazabicyclo (5,4,0) undecene-7, triphenylphosphine, benzyldimethylamine, and 2-methylimidazole.

The following components can be added to the resin composition of the present invention as needed. That is, as the low stress agent, silicone rubber, polysulfide rubber, acrylic rubber, butadiene rubber, styrene block copolymer, or the like, rubber-like substances such as saturated elastomers, various thermoplastic resins, and the like. Further, apart from the silane coupling agent used for the surface treatment of the spherical silica powder, γ-
Glycidoxypropyltriethoxysilane, β- (3,
4-epoxycyclohexyl) ethoxysilanes such as ethyltrimethoxysilane, aminopropyltriethoxysilane, aminosilanes such as N-phenylaminopropyltrimethoxysilane, hydrophobic silane compounds such as methyltrimethoxysilane, octadecyltrimethoxysilane,
Examples of the surface treatment agent include a titanate coupling agent and an aluminum coupling. Further, as a flame retardant auxiliary, Sb ₂ O ₃ , Sb ₂ O ₄ , Sb ₂ O _5, etc., as a flame retardant, halogenated epoxy resin, phosphorus compound, etc.
Colorants include carbon black, iron oxide, dyes, pigments and the like. A release agent such as wax can be added.

When the resin composition of the present invention is solid, the above-mentioned materials are mixed by a blender or a mixer, and then melt-kneaded by a heating roll, a kneader, a single- or twin-screw extruder, a Banbury mixer, etc., and cooled. It can be manufactured by crushing later. In the case of a liquid, the above-mentioned various materials can be prepared by mixing at room temperature or by heating with a universal stirrer, a three-roll mill, a kneader, or the like, followed by defoaming.

In the present invention, the average particle diameter is determined by a laser scattering method, for example, a particle size analyzer (model LS manufactured by Coulter Inc.).
-230). When measuring,
It is desirable to perform ultrasonic dispersion using pure water to which a suitable amount of a dispersant such as sodium hexametaphosphate is added as a dispersion medium. The specific surface area is measured by a BET method, for example, a specific surface area measuring device (model 4-SORB) manufactured by Yuasa Ionics.

The average sphericity can be measured using a field emission scanning electron microscope (“JSM-6301F” manufactured by JEOL Ltd.) and an image analyzer (manufactured by Nippon Avionics Co., Ltd.) as follows. First, the projected area (A) and the perimeter (PM) of the particles are measured from the SEM photograph of the powder. Assuming that the radius of a perfect circle corresponding to the perimeter (PM) is r, PM
= 2πr, so that r = PM / 2π. Assuming that the area of the perfect circle assumed above is (B), B = (PM) ²
/ 4π. Here, since the sphericity of a particle is calculated as A / B, the sphericity of each particle is represented by sphericity = A /
B = A × 4π / (PM) ² . Therefore, the average sphericity was determined by averaging the sphericity of 200 arbitrary particles.

The decrease rate of the average sphericity is calculated by the following equation. For example, if the average sphericity of the raw silica powder having an average sphericity of 0.90 after the surface treatment is 0.88, the sphericity reduction rate is calculated as 2%. Reduction rate of sphericity (%) = (| average sphericity of raw silica powder−average sphericity of treated powder |) × 100 / average sphericity of raw silica powder

The silanol group concentration is determined by the Karl Fischer method, for example, a micro-moisture analyzer (Model C, manufactured by Mitsubishi Chemical Corporation).
It can be measured from the moisture value according to A-05). In this measurement method, fine spherical silica powder was set in a quartz tube in a moisture vaporizer, and argon gas dehydrated was supplied as a carrier gas while heating with an electric heater, and silanol groups attached to the surface of the raw material silica powder were removed. The water vapor condensed and volatilized can be obtained by guiding the water vapor to a measuring instrument and measuring the water content. In the present invention, the water generated up to a heating temperature of less than 250 ° C. is considered as physically adsorbed water, and the water generated up to a heating temperature of 250 to 900 ° C. is dehydrated and condensed with silanol groups.
The silanol group concentration per unit surface area was determined.

[0040]

The present invention will now be described more specifically with reference to examples and comparative examples.

Example 1 Raw material silica powder (average sphericity: 0.90, average particle diameter: 0.1
1.5 kg of 3 μm, specific surface area of 16 m ² / g, surface silanol group concentration of 5.0 particles / nm ² ) was charged into a vibrating fluidized bed apparatus (“VUA-20” manufactured by Chuo Kakoki), and the amplitude was 2 m.
m, frequency: 1500 rpm, air volume 230 L / min
In a state of fluidization under the conditions described above, 22 g of γ-glycidoxypropyltrimethoxysilane (equivalent to 30% of the specific surface area of the raw silica powder) was mixed for about 10 minutes while spraying. Further, after mixing for 20 minutes, the treated powder was taken out and sieved at 140 μm to produce the finely-surface-treated fine spherical silica powder of the present invention.

Examples 2 to 4 Comparative Examples 1 to 3 Production was carried out in the same manner as in Example 1 except that the amount of the silane coupling agent added was changed to the ratio shown in Table 1.

With respect to the fine spherical silica powders obtained in Examples 1 to 4 and Comparative Examples 1 to 3, the agglomeration amount of> 25 μm, the viscosity, the reduction rate of the sphericity after the treatment, and the dispersibility at the time of filling the liquid epoxy were as follows: It measured according to the following. Table 1 shows the results.

Examples 5 to 8 Comparative Examples 4 to 7 The fine spherical silica powders of Examples 1 to 4 and Comparative Examples 1 to 3 were mixed at the ratios shown in Tables 2 and 3 to prepare a slurry.
It was poured into a mold and cured by heating, and the flexural strength of the obtained cured epoxy resin was measured. Tables 2 and 3 show the results.

Examples 9 to 11 Comparative Examples 8 to 10 The fine spherical silica powder obtained in Example 4 and a base inorganic powder (spherical fused silica powder, “FB-
820 ”(average particle size: 25 μm) at a ratio shown in Tables 4 and 5 to prepare an inorganic filler. According to the formulations shown in Tables 4 and 5, a resin composition was prepared, and its fluidity, bending strength and solder heat resistance were evaluated. Tables 4 and 5 show the results.

(1) Carbon content 10 g of fine spherical silica powder is added to 100 g of acetone and stirred for 30 minutes. Thereafter, the slurry liquid is separated into fine spherical silica powder and acetone by a centrifugal separator, and the supernatant solution of acetone is discarded. This washing operation with acetone is performed three times and dried at 70 ° C. for 1 hour. Next, a carbon / sulfur simultaneous analyzer “CS-444LS type” (manufactured by LECO) was measured for carbon content in 0.5 g of the washed fine spherical silica powder.
And quantified by the calibration curve method.

(2) Aggregation Amount 20 g of the fine spherical silica powder was subjected to water sieving for 1 minute with a shower having a flow rate of 12 L / min with a sieve having an opening of 25 μm and dried on the sieve at 150 ° C. × 2 hours. The obtained mass was calculated as a ratio (%) to the total mass of the sieve.

(3) Viscosity 0.5 cm ^{3 of} the slurry used for the evaluation of dispersibility was placed in a measuring holder of an E-type viscometer “Model EHD” (manufactured by Tokyo Keiki).
After filling, was measured at 25 ° C. with a rotor having an angle of 3 ° at a shear rate of 20 / s.

(4) Dispersibility Alicyclic liquid epoxy resin "Araldite CY179"
After adding 30 g of fine silica powder to 70 g (manufactured by Ciba Specialty Chemicals Co., Ltd.), the number of revolutions was 600 rpm using a simple kneader “Awatori Nerita AR-360M”.
The mixture was kneaded for 10 minutes under the conditions of m and the number of revolutions of 2000 rpm, and the presence or absence of the aggregation state was visually confirmed. ：: No easily detectable aggregated particles were observed. Δ: Less than 10 aggregated particles having a size that can be easily detected are observed. ×: 10 or more aggregated particles having a size that can be easily detected are observed.

(5) Fluidity (Spiral Flow) Using a spiral flow mold, the spiral flow was measured according to EMMI-66. The molding temperature is 175 ° C,
The molding pressure was 7.4 MPa.

(6) Flexural strength The resin composition was heated at a mold temperature of 180 ° C. at 4 mm × 16 mm ×
After molding into a size of 80 mm and post-curing at 180 ° C. for 6 hours, it was measured according to the bending strength measurement method of JIS K 6911.

(7) Solder heat resistance (number of cracks generated) 16 low-pressure transfer molding methods were used to obtain 16 44-pin QFP molded bodies (packages) encapsulating the simulated device under the conditions of 175 ° C. × 2 minutes, and then 175 ° C. Post-curing was performed for × 5 hours. These were left for 96 hours at a temperature of 85 ° C. and a humidity of 85 RH%, immersed in solder at 260 ° C. for 10 seconds, and the number of internal cracks observed in the 16 compacts was measured by an ultrasonic probe. Examined.

[0053]

[Table 1]

[0054]

[Table 2]

[0055]

[Table 3]

[0056]

[Table 4]

[0057]

[Table 5]

[0058]

The fine spherical silica powder of the present invention has an average particle diameter of 1.0 μm or less and an average sphericity of 0.85 or more, and the average sphericity does not deteriorate before and after the surface treatment. Even when a solid or liquid resin is filled at a high level, alone or in combination with a base inorganic powder, the dispersibility and fluidity are not deteriorated, and the heat resistance of the semiconductor resin sealing material and the like can be remarkably improved.

That is, according to the present invention, even if the resin composition is a resin composition in which the filler is highly filled, the fluidity of the resin composition and the reliability of the molded product can be greatly improved without impairing the dispersibility. Provided are a fine spherical silica powder which can be improved, and an inorganic filler and a resin composition using the same.

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Claims (6)

[Claims] An average particle size of 1.0 μm or less and an average sphericity of 0.85 or less, which has been surface-treated with a silane coupling agent.
The above silica powder, wherein the amount of the silane coupling agent is 30 to 70% of the specific surface area of the raw silica powder,
A fine spherical silica powder having a carbon content of 0.05 to 5%. 2. The silane coupling agent according to claim 1, wherein the silane coupling agent has three alkoxy groups, and the organic functional group directly bonded to Si has 1 to 10 carbon atoms. Fine spherical silica powder. 3. A silane coupling agent is spray-sprayed on a fine spherical silica powder raw material having an average particle diameter of 1.0 μm or less and an average sphericity of 0.85 or more, which is highly dispersed by a vibrating fluidized bed. The method for producing a fine spherical silica powder according to claim 1. 4. An inorganic filler comprising 3 to 30% of the fine spherical silica powder according to claim 1 or 2. 5. A resin composition comprising 10 to 40% of the fine spherical silica powder according to claim 1 or 2. 6. The method according to claim 4, wherein the inorganic filler is 70 to 9%.
A resin composition comprising 5%.