JPS59189139A - Inorganic sphere and resin composition containing the same - Google Patents

Abstract

PURPOSE:To provide an inorg. sphere which has excellent flow characteristics, fillability, warkability, etc., is suitable for use as a filler for resins, and contains little alkali ions which can be leached with warm water, by forming a fused quartz layer on the surface of a fine particulate core. CONSTITUTION:The titled inorg. sphere has at least a surface layer composed of fused quartz and a particle size of 500mu or below and contains alkali ions in such a quantity that the quantity of the alkali ions leached out after immersing it in warm water at 90 deg.C for 24hr is 10ppm or below. The inorg. sphere can be prepd. in such a manner that a core (e.g. sintered alumina) having a particle size of 500mu or below and a low alkali compd. content is mixed with colloidal silica, the mixture is dried, the dried material from the central raw material feed tube 2 of the oxyhydrogen burner 5 of a flame spray furnace 6 together with a combustible gas 3 (e.g. hydrogen or acetylene) and oxygen 4 is flame-sprayed into the flame spray furnace 6 to heat it at a high temp. and then cooled.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention provides a fine powder inorganic spherical body and a resin composition thereof, and furthermore, the present invention relates to a finely powdered inorganic spherical body and a resin composition thereof, and a particle size of 5.
The present invention relates to an inorganic spherical body and an inorganic spherical body whose alkali ions extracted by immersion in hot water at a temperature of 90° C. for 24 hours are 00μ or less and 1 ppm or less, and a fat composition thereof.

Conventionally, glass beads, alumina, etc. have been known as filling materials for hard resin.

However, all of these contain fJ]O% of alkaline compounds such as Na2O and 20, and when these are blended into thermosetting resins, the alkali compounds such as Na2Q and 20 in the filler material become alkali ions. Therefore, when such a fat composition is used as a material for electronic parts, it has the drawback of causing damage to the P-scale and corrosion.

1* UIC and LSI that are made by blending inorganic powder such as crystalline quartz, fused quartz, and sintered alumina with thermosetting resin
It is used as a sealing material for electronic components and an insulating material for electrical components. However, since the inorganic My powder is a pulverized product obtained by pulverizing the agglomerates to a predetermined size,
Because its shape is not perfectly spherical and has corners, when it is blended with thermosetting 4W chive resin to make a sealing material, its fluidity is insufficient, making it difficult to fill and work. When molding, there is a drawback that equipment such as mixers and molding machines suffers from severe wear.

The present invention aims to provide an inorganic spherical body that solves these drawbacks and a resin composition containing the same.

That is, in the first aspect of the present invention, at least the surface is made of fused silica and the maximum particle size is 500μ or less. ] Oppm or less, and the second invention is made of particles whose surface is made of fused silica and whose maximum diameter is 500μ or less, and which is immersed in hot water at a temperature of 90°C for 24 hours. This is a molded piece resin composition in which the resin composition contains 30 to 80% by weight of inorganic spherical bodies whose extracted alkali ions are not more than Oppm.

The present invention will be further explained in detail below.

First of all, the first invention provides good fluidity when blended with synthetic resin, and also has a maximum particle size of 5 that can be blended into synthetic individual fat.
This is an inorganic 54 spherical chamber with little elution of alkali ions of 00μ or less.

The spherical body of the present invention has at least a surface of 5t0299, 5
It is formed from fused silica with an alkali ion content of 100 ppm or more, and its maximum particle size is 5.
Not only those in which all single particles of 00μ or less are made of fused silica, but also crystalline quartz or materials that form intermolecular compounds with silica such as alumina, magnesia, zurconia, and spinel, or mullite (3A12037・2&Ot),
Cordierite (190,・2A6,03.A・5S is also 02), Zircon fZ+:02.・5cCh) Includes those in which particles of intermolecular compounds such as carbonate and silica are used as a core material, and a layer of bath-fused quartz is formed on the surface thereof. Furthermore, since the surface of the inorganic spherical bodies of the present invention is made of fused silica, unlike conventional pulverized products, the inorganic spherical bodies have a smooth surface and are almost spherical in shape, with a particle diameter ratio of 1 to 2 when observed under a microscope. It consists of single particles with a maximum particle size of 500 μm or less. If the maximum particle size exceeds 500 μm, it is not preferable because there are problems such as the compounded and mixed spherical bodies settling in the resin.

To produce the product of the present invention, each of Na2O and Ni20 is preferably 0.01% by weight or less, more preferably 0.05% by weight.
A method in which high silicic acid powder of the following silica stone or silica sand with a particle size of 500 μm or less is ejected simultaneously with fuel gas and acid accumulation, and is instantaneously melted to form a molten stone into a spherical body, and then cooled and collected, or the content of alkali compounds After mixing and drying an aqueous slurry such as colloidal silica white carbon or silica glue to the core material so that the solid content is 30% by weight or less, preferably 2 to 20% by weight, the same method as described above is carried out. can get.

In addition, the product of the present invention must be immersed in hot water at a temperature of 90°C for 24 hours, and the amount of alkali ions extracted into the hot water must be 10 ppm or less, preferably 5 ppm or less, and if the amount exceeds 1 Oppm. When this is blended into a resin, the amount of alkali ions liberated and accumulated in the resin increases, which is undesirable because it leads to dielectric breakdown and corrosion of processed products.

Next, the second invention of the present invention will be explained.

This invention is a resin composition containing 30 to 80% of the inorganic F7 spherical bodies of the first invention.

Specific examples of resins used as base materials in the present invention include curable resins such as epoxy resins, phenolic resins, polyester resins, and silicone resins, and thermoplastic resins such as polyethylene, polypropylene, and 12-listyrene.

In addition, the inorganic spherical bodies are contained in the resin composition in an amount of 30 to 80% by weight.
However, if it is less than 30% by weight, it will not have excellent electrical insulation properties, and if it exceeds 8% by weight, the proportion to the prime resin will be large and molding will be difficult.Resin composition according to the present invention The product can be obtained by kneading the Primer resin, unmixed powder, and various additives depending on safety using a roll, kneader, mixer, Banbury mixer, etc.

As explained above, the first aspect of the present invention is an inorganic spherical body whose surface has a particle size of 500 μm or less from which alkali ions are less eluted, and which extracts fewer alkali ions than conventional products. The effect is that the surface has no corners and is half-shaped.

The present invention will be explained below with reference to Examples.

Examples and comparative examples The inorganic spheres shown in Table 1 were produced as follows.

The furnace used was an apparatus having a diameter of 20 ann and a height of 200 cm as shown in FIG. 1.

The raw material is silica (5tCh 99.5%, Le 2030
．． 063%, Fb2030.002%, Na2O0,
002%, K2O0,003%) was ground in a ball mill to a particle size of 44μ or more. Insert all of this into the Hola Gu-IVc as shown in Figure 1, and then use a constant feeder for 10~/
The raw material was continuously supplied into the furnace from the central raw material supply pipe 2 of the oxyhydrogen burner 5.

As combustible gases, hydrogen was supplied into the furnace from a hydrogen gas blowpipe 3 and oxygen gas was supplied from an oxygen gas blowpipe 4.

The raw material 1 melted by the flame descends into the furnace body 6, is sucked up by the blower 10, passes through the transport pipe 7, and is transferred to the cyclone 8,
It was collected on a grasshopper filter 9.

In addition, hydrogen gas is 30 Nm'/Hr (43.9m/
see) Oxygen gas 15 Ntr? /'Hr (8,3
m/sec), gas flow rate ratio (H2/0215.2
It was conducted under the following conditions.

The burner shown in FIG. 2 was used. In addition, in Fig. 2, 2 is a raw material supply pipe, 3 is a hydrogen supply pipe, and 4 is an oxygen supply pipe, and their cross-sectional areas are 0.5 crA and 1.97, respectively.
s 5-0 was used. FIG. 3 shows an electron microscope 4 of the granular material produced in this manner.

(B) Fused silica using sintered alumina as the core material. Commercially available colo-glue with a low alkali content υ′/J is defined as 1° weight based on 100 parts by weight of commercially available sintered alumina with a particle size of 500μ or less. % and mixed with a mixer and dried. This is described above (Al 7
The same method as that for manufacturing 8 fused silica spheres was carried out.

(C) Crushed fused silica 5if299.9% Na2o Oll 01% K2O
0.002% sandstone powder was bath-melted and ground in a total melting furnace.

(D) Pulverized sintered alumina Commercially available sintered alumina was completely crushed.

-23'.

(2) Production of resin composition 100 parts and 38 parts by weight of thermosetting resin composition 1/sol 7 nopora ivy type evo/r position January effect, phenol no yje lac position April effect, and carnauba wax, respectively. and 2 parts, totaling 140 parts, while the inorganic powder was used at the J-eel ratio shown in Table 2 VC. In addition, M rat% in Table 2
i: Indicates the proportion in the composition.

These were heated to a temperature of 80 to 100°C, homogeneously kneaded with an 8-inch mixing roll for about 10 minutes, cooled, and ground to a temperature of 160°C.
Transfer molding was performed at ℃, pressure cuff 0KI/v, and moxibustion conditions of 4.

The physical properties of each of these are defined and shown in Table 3.

, /' 2, /'/' / / / / , 7/ / / / / / / / / 239- (1) Measurement of fluidity (spiral flow) Using a mold that complies with EMMI standards, molding temperature 160°C , molding pressure cuff 0
To? Measured at /-.

(2) Measurement of resin stress A male resistor whose resistance value changes depending on the stress is molded into a semiconductor chip, and is tied to a 14-bin IC frame, and connected to the external electrode by connecting it to the external electrode using the AU wire. The initial resistance value (Ro) was measured and the device was heated at 160°C for 7
Resistance (R)t after resin sealing under the conditions of 0Kp/-molding time of 3 minutes, (R-Rh)/Rok Ij
It was defined as fat stress.

[Brief explanation of drawings]

Fig. 1 is a schematic explanatory diagram of the device according to the embodiment of the present invention, Fig. 2 is a sectional view of the burner, Fig. 3 is an electron micrograph of the inventive product (A), and Fig. 4 is an electron micrograph of the comparative product (C). be. 3. Combustible gas blowpipe, 4.-- Oxygen gas blowpipe,
5. Burner, 6. Furnace body, 7. Transport pipe, 8. Cyclone, 9. Back filter, 10 Prower 6 Applicant Electrochemistry]
− Business Co., Ltd. Procedures Sode′ Masa Kutsu (Ka style)
August 5, 1980 1J Director General of the Patent Office Wakasugi +11 people ■, Indication of Inno J 1988 Patent Application No. 62651 Title of the invention Inorganic spherical bodies Js and their resin compositions, person making the amendment Relationship with tenant farming Tokushi'1 Applicant Address 1-J114-1 Jirakucho, Chiyo 111-ku, Tokyo
Name (329) Contents of Denki Kagaku Kogyo Co., Ltd. 4th Amendment

Claims (1)

[Claims] ]) At least the surface is made of fused silica and the grain size is 50.
Alkali ions produced by substances with a particle size of 0μ or less and extracted by soaking in hot water at a temperature of 90℃ for 24 hours] Op
Inorganic spherical bodies with a particle size of pm or less. 2) At least the surface is made of #fused silica and the grain size is 50
The alkali ions that are made up of substances with a diameter of 0 μ or less and that are extracted by soaking in hot water at a temperature of 90°C for 24 hours are l Op.
30 to 8 pm or less of inorganic spherical bodies in the resin composition.
() A resin composition containing % by weight.