JPH02245011A - Highly pure phenolic resin, composition containing same, its production, and electronic device made from the same resin - Google Patents

Abstract

PURPOSE:To obtain the title resin excellent in moldability, adhesiveness, electrical properties, etc., by adding an organic solvent to a resol phenolic resin obtained by the condensation of a phenolic compound with HCHO and subjecting the mixture to a specified washing treatment with deionized water. CONSTITUTION:An organic solvent (e.g. acetone) is added to a resol phenolic resin obtained by the condensation of a phenolic compound with HCHO, and the mixture is subjected to a washing treatment with deionized water (e.g. ion-exchanged water). This washing treatment is repeated until an extract obtained by extracting the treated resin with hot water of 120 deg.C in an amount of at least 10 folds in wt. resin for 100hr or longer has an electrical conductivity <=100muS/cm, a pH of 3-7 and a halide ion content and an ammonium or metallic incontinent each of which is 10ppm or below.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to high purity phenolic resin, and particularly to moldability,
The present invention relates to a high-purity phenol resin that provides a phenol resin composition with excellent adhesiveness, electrical properties, and heat resistance, the resin composition, and an electronic device using the resin.

[Conventional technology]

Depending on the purpose, thermosetting resins such as phenol resin, unsaturated polyester resin, epoxy resin, silicone resin, polyimide resin, nylon, polyacetal, polycarbonate, etc. are used as insulation, adhesive, and structural materials for electronic devices and electrical equipment. Thermoplastic resins such as polyester, polysulfone, polyethersulfone, polyamideimide, and fluororesin are used.

However, in resin-sealed semiconductor devices and multilayer printed circuit boards that require a high degree of reliability, most of the resins used are epoxy resins, silicone resins, and polyimide resins.

In particular, more than 80% of semiconductor products such as transistors, ICs, LSIs, and VLSIs are resin-sealed products that are transfer-molded using thermosetting resins, mainly epoxy resins.

The degree of integration of the semiconductor chips of the above-mentioned semiconductor products is increasing year by year, and along with this, the chip size is increasing, the wiring is becoming finer, and the number of layers is increasing.

Along with the above, the surfaces of semiconductor chips are becoming more delicate, and the sealing resin layers are gradually becoming thinner.

Furthermore, with the shift from the bottle insertion type to the surface fabrication type, the packages are exposed to higher temperatures (200° C. or higher) than before during mounting. Therefore, cracking of the sealing resin, semiconductor chip, or passivation film due to thermal stress has become a problem.

[Problem to be solved by the invention]

In recent years, as the usage conditions for electronic devices and electrical equipment using such resins have become stricter, requirements for safety have become even more stringent, and higher heat resistance, flame retardance, and durability are required.

For example, halogen-based or phosphorus-based compounds are used as flame retardants to make epoxy resins flame retardant. However, since these flame retardants have a relatively low thermal decomposition temperature, they are thermally decomposed by heating during molding, and the decomposition products deteriorate the electrical properties.

In particular, the decomposition products of halogen-based flame retardants are a problem because they contain harmful substances.

The present invention was created in view of these circumstances, and its objectives are to improve moldability and adhesion.

The present invention provides a high-purity phenol resin that has good electrical properties, moisture resistance, heat resistance, etc., and has excellent properties particularly as a sealing material for electronic devices, electrical equipment, etc., the resin composition, and a method for producing the same.

[Means to solve the problem]

Conventionally, phenolic resins have a high content of ionic impurities, and when cured or when the cured product is exposed to high temperatures,
It was considered almost impossible to put it to practical use as a material for electronic components because it generates free phenol and ammonia gas, which corrodes surrounding metal materials and degrades electrical properties.

The present inventors focused on the fact that phenolic resin has excellent flame retardancy, and investigated the improvement of its electrical properties and its applicability to molding materials.

As a result, resol-type phenolic resin was surprisingly able to improve the above-mentioned properties through high-purity purification.
In particular, it has been found that when used for encapsulating semiconductor devices, there is no adverse effect on the soldering heat resistance of the semiconductor device or the reliability of the joint between the gold wire and aluminum electrode even when heated at high temperatures for long periods of time. I came up with an invention.

The gist of the present invention is as follows.

(1) Add an organic solvent to a resol-type phenolic resin obtained by condensing a phenolic compound and formaldehyde, wash it with pure water, and soak the treated resin in 10 times the amount of hot water at 120°C for more than 100 hours. The electrical conductivity of the heated extract is less than l O O p S / cm, p
A method for producing a high-purity phenol resin, characterized in that the washing treatment is repeated until H is 3 to 7 and the amount of halogen ions, ammonium ions, or metal ions is each 10 ppm or less.

(2) The method for producing a high-purity phenolic resin according to the above item (1), wherein the resol type phenolic resin has a number average molecular weight of 400 or more, and the unreacted phenol in the resin is 1% by weight or less.

(3) The resol type phenol resin that has been washed with an organic solvent and pure water is washed with 10 times the amount of hot water at 120'C.
The electrical conductivity of the extract extracted by heating for more than 0 hours is 1 0
A high-purity phenol resin characterized by having a phenolic resin of 0 pS/cm or less, a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions of 10 ppm or less.

(4) The high-purity phenolic resin according to item (3) above, wherein the resol type phenolic resin has a number average molecular weight of 400 or more, and the unreacted phenol in the resin is 1% by weight or less.

(5) The resol type phenolic resin has the following general formula [1
], and 10 times the amount of the resin.
The extract extracted by heating with hot water at 20°C for 100 hours or more has an electrical conductivity of 100 μS/Qm or less, a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions each of 10 PPm or less. High purity phenolic resin.

[In the formula, R represents H, -CH20H or =9-, provided that at least 10 H2-0-CH2 is included. n represents a number from 3 to 10. ] (6) A resol type phenol resin obtained by condensing a phenol compound and formaldehyde, and a
An organic solvent is added to a resin composition containing 5 to 5% by weight of epoxy resin, followed by washing with pure water, and the treated resin is washed with 10 times the amount of hot water at 120°C. O
The electrical conductivity of the extract extracted by heating for more than 0 hours is 100.
The cleaning process is repeated until pS/cm or less, pH is 3 to 7, and the amount of halogen ions, ammonium ions, or metal ions is each 10 ppm or less to remove the organic solvent and water. A method for producing a high purity phenolic resin composition.

(7) The resol type phenolic resin has a structure represented by the general formula (N), and the resin is added to 120
The extract extracted by heating with hot water at ℃ for 100 hours or more has an electrical conductivity of 100 μS/Qm or less, a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions of 10 ppm or less each. The method for producing a resin composition according to item (6) above, characterized in that the resin composition is a pure phenolic resin.

(8) A resol-type phenolic resin composition containing 25 to 5% by weight of epoxy resin that was washed with an organic solvent and pure water was heated and extracted with 10 times the amount of hot water at 120°C for more than 100 hours. The electrical conductivity of the extract is 100μS/
cm or less, pH 3-7, amount of halogen ions, ammonium ions or metal ions each IQppm
A high purity phenolic resin composition characterized by the following:

(9) The resol type phenolic resin has the general formula [I]
The resin composition as described in the preceding item (8), which has a structure shown in the following.

(10) An electronic device sealed with the resin or resin composition according to any one of (3), (4), (5L) (8) and (9).

(11) A semiconductor device sealed with the resin or resin composition according to any one of (3), (4), (5), (8), and (9).

The resol type phenolic resin of the present invention is synthesized by a condensation reaction of various phenols and aldehydes in the presence of an amine or an alkali catalyst, an organic metal salt, etc. After the reaction, unreacted raw materials and ions are removed. To remove sexual impurities.

The desired high-purity phenol is obtained by dissolving the condensate in an organic solvent, adding a large amount of pure water to this solution, stirring vigorously, allowing it to stand, and then repeating the washing process to remove the supernatant. Resin can be obtained.

A rough guide to purity is to dissolve the resin in 10 times the amount of hot water at 120°C.
The electrical conductivity of the extract extracted by heating for more than 00 hours is 100.
pS/cm or less, pH is 3 to 7, and the amount of halogen ion, ammonium ion, or metal ion is each 1 oppm or less.

According to the present inventors, it has been confirmed that resol type phenolic resin can be highly purified by simply washing with pure water.

However, in that case, it is necessary to increase the number of cleaning treatments. From an industrial standpoint, it is preferable that the number of times of washing treatment be small.

The present invention is characterized in that an organic solvent is used to improve this cleaning effect. This makes it possible to reduce the number of cleaning treatments by about half compared to cleaning treatments using only pure water.

In particular, the electrical insulation property of the cured product, which is the biggest drawback of phenolic resin, is 1014 Ω when washed only with pure water.
Cm (uncleaned: 1010Ωam) order, whereas when using the organic solvent of the present invention, xo14ΩQ
m or more.

Furthermore, since metal salts and the like are removed at the same time, thermal deterioration is less likely, and the weight loss rate due to heating at 250° C. is 20 to 30% less than when cleaning using only pure water.

In the present invention, a specific example of the organic solvent used for the cleaning treatment is not particularly limited as long as it can dissolve the resol type phenolic resin, but it is preferable to use a solvent that is compatible with water.

Specific examples of the organic solvent include acetone, tetrahydrofuran, methyl ethyl ketone, hexane, cyclohexane, ethyl acetate, dioxane, methyl isobutyl ketone, and the like. Solvents with high boiling points are not preferred because they are difficult to remove later.

The amount of solvent used should be the amount necessary to dissolve the resin, but
It is best to add the same amount as the resin or a little more.

The above-mentioned resol type phenolic resin can be synthesized by condensation reaction of phenol or phenols such as cresol with formalin in the presence of a catalyst such as an amine or an alkali MW or an organic metal salt, but the curability and fluidity of the resin From the relationship, it is desirable to set the reaction conditions so that the number average molecular weight is 400 or more.

The amines used in the above catalysts include ammonia, dimethylamine, diethylamine, aniline, hexamethylenetetramine, triethylamine, and triethanolamine, and the alkali catalysts include sodium hydroxide, potassium hydroxide, calcium hydroxide, and hydroxide. Magnesium, barium hydroxide, calcium oxide, magnesium oxide, etc.

Examples of organic metal salts include metal salts of aliphatic carboxylic acids such as zinc acetate, copper acetate, iron acetate, lead acetate, magnesium acetate, calcium acetate, barium acetate, nickel acetate, cobalt acetate, cadmium acetate, zinc benzoate, Examples include metal salts of aromatic carboxylic acids such as zinc phthalate.

Note that in order to remove unreacted raw materials and ionic impurities, it is effective to use neutralization treatment using an acid or steam distillation in combination with the above-mentioned cleaning treatment.

The thus obtained resol type phenolic resin of the present invention has a reactive methylol group, dimethylene ether group, and hydroxyl group in the molecule, so that it can be cured by heating alone. Moreover, its reactivity is considerably faster than that of epoxy resins even when no curing catalyst is used.

In particular, among the resol type phenolic resins represented by the general formula [I], the dimethylene ether represented by R2 (
Those having many -CH, -0-CH2-) bonds produce less condensed water during curing, and therefore provide excellent properties as a cured product.

For this purpose, in general formula (1), it is necessary that 20% or more of all R2 be -CH2-0-CH,-.

In the high-purity resol type phenolic resin of the present invention, it is desirable that the unreacted phenol content in the resin is 1% by weight or less. This level of unreacted phenol does not pose a problem since it will react during curing.

Furthermore, the high purity phenol resin of the present invention can also be cured with epoxy resin or maleimide resin. In particular, in order to fully achieve the object of the present invention, the electrical properties of the cured product can be further improved by using a well-known epoxy resin as a curing agent. In this case, 25 to 5% by weight of epoxy resin (curing rate control agent) is blended with 75 to 95% by weight of resol type phenolic resin. If the epoxy resin is added in an amount exceeding 25% by weight, the flame retardancy of the cured product will decrease, which is not preferable. on the other hand.

If the amount is less than 5% by weight, the effect of the epoxy resin formulation cannot be sufficiently obtained.

The above-mentioned epoxy resin is a well-known resin obtained by a condensation reaction of bisphenol A or phenol novolac resin and shrimp chlorohydrin. It goes without saying that unreacted raw materials and ionic impurities must be sufficiently removed from the epoxy resin.

The ionic impurities contained in these resin components are similar to the case of the phenolic resin of the present invention, and when the resin is extracted with 10 times the amount of 120°C hot water for 100 hours or more, the electrical conductivity of the extracted liquid increases. 100μS/am or less, pH 3-7,
The amount of extracted halogen ions, ammonium ions, or metal ions must be 10 ppm or less.

The high purity phenol resin and high purity phenol resin composition of the present invention may contain an inorganic filler.

The inorganic filler is added for the purpose of improving the coefficient of thermal expansion, thermal conductivity, modulus of elasticity, etc. of the cured product, and is preferably used in an amount of 55 to 80% by volume based on the entire resin or composition.

If it is less than 5S by volume, the above characteristics cannot be sufficiently improved, and if it is added in excess of 80 volume%, the viscosity of the material will increase significantly and the fluidity will decrease.
It is best to mix them according to the purpose. Although there are various inorganic fillers, it is especially important to use thermally and chemically stable fillers for electronic components. Specifically, fused silica, crystalline silica, alumina, etc. are desirable.

Spherical fused silica, which has recently been mass-produced industrially, is useful because it has a small coefficient of thermal expansion, and when mixed with resin, there is little increase in viscosity or decrease in fluidity of the composition. be.

Note that the average particle size of the filler is preferably 1 to 30 μm. If it is less than 1 μm, it increases the viscosity of the resin composition and significantly reduces the fluidity.

In addition, if it exceeds 30 μm, the resin and filler will easily separate during molding, forming an uneven layer within the cured product, resulting in variations in the properties of the cured product and poor filling properties into narrow gaps. I don't like it because it has harmful effects.

The high-purity phenolic resin of the present invention or the composition may optionally contain a curing catalyst for accelerating the curing reaction of the resin, a plasticizer for toughening the cured product and lowering the elastic modulus, and a resin. The purpose of the present invention is to add various additives such as a capping agent to improve adhesion to fillers, dyes and pigments for coloring, and a mold release agent to improve release properties from a mold during curing molding. They can be used together within a range that does not impair the properties.

Similarly, if fillers and these various additives contain large amounts of ionic impurities, the reliability of various products will be significantly reduced. When extraction is performed with hot water for 100 hours or more, the electrical conductivity of the extract is 100μS/
It is necessary that the pH is 3 to 7, and the amount of extracted halogen ions, ammonium ions, or metal ions is 10 ppm or less.

In addition, in order to reduce the influence of the above-mentioned ionic impurities on various reliability of the product, it is also effective to directly blend ion exchange resin or fine powder of ion exchanger into the resin.

In particular, antimony or bismuth hydroxide, hydrated oxide, phosphorus antimonic acid, zirconium antimonate,
0 so-called inorganic ion exchangers such as titanium antimonate, tin antimonate, chromium antimonate, tantalum antimonate, etc. per 100 parts by weight of the resin or resin composition.
．． By blending 01 to 5 parts by weight, preferably 0.1 to 1 part by weight, corrosion and breakage of aluminum wiring and electrode parts during moisture resistance tests of resin-sealed semiconductor devices, as well as resin-sealed semiconductor devices. It is effective in preventing corrosion and disconnection of the joint between the gold wire and aluminum electrode during high-temperature storage tests.

[Effect]

The reason why the high purity resol type phenolic resin of the present invention has excellent electrical properties and other properties is due to the high degree of purification.
This is because various ionic impurities were removed. Also,
The reason why phenolic resins have excellent heat resistance is thought to be due to the presence of benzene rings and phenolic hydroxyl groups with a high return element content, or the excellent heat resistance of cured resins.

Next, the present invention will be explained by examples.

Example 1 (Synthesis of resol-type phenolic resin) 500 g of phenol, 550 g of 30% formalin + 5 g of zinc acetate as a hardening agent were added to a 5Q flask, and the mixture was gradually heated while stirring, and heated at 90°C for 60 minutes under reflux. The pressure inside the flask was reduced to 20 mmHg to remove condensed water and unreacted components.

Next, as a cleaning treatment, 300 g of acetone was added to the above reaction product to dissolve it, and ion-exchanged water 3Q was added thereto and vigorously stirred at 50°C for 30 minutes. After cooling to room temperature, the upper aqueous layer was removed. Removed. This washing process was repeated seven times.

After each cleaning treatment, a portion of the reaction product was collected and dried by heating at 4.0"C under reduced pressure for 48 hours to obtain unwashed and six types of resol types with different degrees of cleaning treatment. A phenolic resin was obtained.

The number of washing treatments, melt viscosity, and curing properties of the obtained resol type phenolic resin, as well as the pI (, electrical conductivity, and Table 1 shows the analysis results of the extracted ionic impurity concentrations.

As is clear from Table 1, when the resol type phenolic resin is subjected to the above washing treatment five times, the electrical conductivity of the extract becomes approximately 20 pS/cm, and the ionic impurities are extremely small. It can be seen that the effect is significant. On the other hand, when cleaning with only pure water, the content of ionic impurities is higher than when using an organic solvent.

Examples 2 to 7 Resol type phenolic resins subjected to the above washing treatment 5 times (number average molecular weight near 1o, softening 3 degrees near 3°C,
Free phenol content 70.3% by weight), and 0-
Cresol novolak type epoxy resin (softening temperature near 5
℃, epoxy equivalent: 198), 2-
Using phenyl-4-methyl-5-hydroxymethylimidazole, spherical fused silica with an average particle size of 15 μm as a filler, epoxy silane as a coupling agent, montanic acid ester wax as a mold release agent, and carbon black as a coloring agent, They were blended in the proportions shown in Table 2.

Each composition was kneaded for 10 minutes with a 20-inch diameter twin-screw roll (roll surface temperature of about 60°C), and then ground to prepare a molding resin composition.

Comparative Examples 1 to 3 Unpurified resol type phenolic resin (initial stage in Table 1 (unwashed). Number average molecular weight: 550. Softening temperature: 62°C
, free phenol content = 3.2% by weight), and a composition having the blending ratio shown in Table 2 was prepared in the same manner as in Example 2.

Comparative Example 4 0-cresol novolac type epoxy resin (
90 parts by weight of brominated bisphenol A epoxy resin (softening temperature 265°C, epoxy equivalent 394), phenol novolac resin as a hardening agent (softening temperature 25°C) °C, hydroxyl equivalent: 106) 55 parts by weight, 10 parts by weight of triphenylphosphine as a curing accelerator, 470 parts by weight of spherical fused silica with an average particle size of 15 μm as a filler, 10 parts by weight of antimony dioxide as a flame retardant aid, A composition containing 3.0 parts by weight of epoxy silane as a coupling agent, 10 parts by weight of montanic acid ester wax as a mold release agent, and 10 parts by weight of carbon black as a coloring agent was prepared using a twin-screw roll in the same manner as in Example 2. The mixture was kneaded to prepare a molding resin composition.

Comparative Example 5 0-cresol novolac type epoxy resin (
Softening temperature near 5°C, epoxy equivalent 195) 100 parts by weight, phenol novolak resin as a hardening agent (softening temperature =
65°C, hydroxyl equivalent: 106) 58 parts by weight, 10 parts by weight of triphenylphosphine as a curing accelerator, 480 parts by weight of spherical fused silica with an average particle size of 15 μm as a filler,
Flame retardant = 5 = 10 parts by weight of antimony dioxide as an agent, 3.0 parts by weight of epoxy silane as a coupling agent, 1.0 parts by weight of montanic acid ester wax as a mold release agent, 10 parts by weight of carbon black as a coloring agent. The blended composition was kneaded using a twin-screw roll in the same manner as in Example 1 to prepare a molding resin composition.

Moldability of each resin composition of Examples 2 to 7 and Comparative Examples 1 to 5, mold temperature 180°C, pressure cuff 0 kg/c
Comparisons were made regarding various properties of molded products that were molded at m2 for 90 seconds and post-cured at 180° C. for 6 hours.

Furthermore, 50 mQ of ion-exchanged water was added to 5 g of powder obtained by pulverizing the molded product into 100 meshes or less, and the various properties of the water after heating at 120° C. for 120 hours were compared. Second result
They are summarized in the table.

From Table 2, it can be seen that the cured products of Examples 2 to 7 using the high-purity resol type phenolic resin of the present invention were higher than those of Comparative Examples 1 to 3 using unpurified resol type phenolic resin. It can be seen that the electrical properties are excellent and the amount of ionic impurities extracted is extremely small.

Furthermore, when compared with the conventional epoxy resin shown in Comparative Example 4.5, the moldability is almost the same, but the heat resistance (glass transition temperature, high temperature bending strength) of the cured product is extremely superior. I understand that.

Furthermore, the molding resin compositions shown in Examples 2 to 7, like the epoxy resin composition of Comparative Example 4, have a flame retardant grade of V according to the UL standard, even though they do not contain a broiler flame retardant. -O
can be satisfied.

Table 3 shows the results of reliability tests on semiconductor devices sealed with each of the above resin compositions.

The test semiconductor device has a silicon chip with aluminum wiring formed in a zigzag pattern on its surface, mounted on a copper lead frame, and a gold wire (30 μm in diameter) connected between the aluminum electrode on the chip surface and the lead frame. and sealed with the resin composition.

From Table 3, it can be seen that the products using the resin composition of the present invention have extremely excellent moisture resistance reliability, heat resistance, and package crack resistance during mounting (reflow).

Next, an example in which the resin composition of the present invention is used in an electronic device will be specifically described with reference to the drawings.

FIG. 1 is a sectional view showing the structure of a planar transistor according to the present invention.

A pnp transistor is formed on the surface layer of a silicon semiconductor substrate 1. A silicon dioxide film 2 is formed as an insulator between an emitter, a base, and a collector formed on the surface of the substrate 1, and a base electrode 3 and an emitter electrode 4 are formed of an aluminum vapor-deposited film. The substrate 1 is fixed to the tip of the tab lead 7, bonded with a gold (or aluminum) wire 5, and the element coated and protected with a resin for the undercoat 6 is coated with a high-purity phenol resin composition, including the tip of the tab lead 7. 8. i.transform molding was carried out.

FIG. 2 is a cross-sectional view showing the structure of a semiconductor device having an integrated circuit.

A semiconductor integrated circuit 11 is a package 1 made of ceramic.
A bonding pad 14 fixed on the package 5 and provided around the integrated circuit 11 is connected to an external connection lead terminal 12 of the package by a bonding wire 13. The above integrated circuit 11. The bonding wires 13, external connection lead terminals 12, and bonding pads 14 were undercoated 9 with moisture-resistant polyimide, and further sealed with a high-purity phenolic resin composition 8.

FIG. 3 is a cross-sectional perspective view showing the structure of a semiconductor memory element.

A memory element 71 made of a silicon chip is fixed to a chip support 72, and an external lead 73 and a memory element 71 are connected to each other.
is connected to the electrode pad 77 by a bonding wire 74. The surface of the memory element was provided with an α-ray shield 176 made of a resin composition containing uranium and thorium of less than IPPb. This was transfer molded with high purity phenolic resin composition 8.

FIG. 4 is a sectional view showing the structure of a semiconductor device having a 27Fl wiring structure on the surface of a semiconductor substrate.

A metal coating is formed on the semiconductor substrate 41 having a silicon dioxide film 42 on its surface, and unnecessary portions of the metal coating are removed by a known etching method to provide a first conductor layer 43 having a desired wiring pattern. .

The conductor layer 43 is electrically connected to the semiconductor element through through holes 48 provided at predetermined locations in the silicon dioxide film 42. Next, the silicon dioxide film 42 is formed by chemical vapor deposition (or a known method such as high frequency sputtering).
After covering the eyebrows 43, through holes 49 were formed in the silicon dioxide film at the conductor connection portions.

Next, a film 44 of an aminosilane compound was formed.

Furthermore, a polyimide film 45 is formed, and a predetermined portion of the polyimide film is etched to form the first conductor! Part of 43 was exposed. A second conductor layer 46 is formed on this in the same manner,
A semiconductor device having a two-layer wiring structure was created. Furthermore, the device was coated with high purity phenolic resin composition 8.

All of the electronic devices of the present invention exhibited excellent heat resistance, moisture resistance, and flame retardance.

〔Effect of the invention〕

The present invention is an extremely excellent method industrially because the number of cleaning treatments can be reduced by approximately half by using an organic solvent and water for purifying high-purity phenolic resin.

Furthermore, the high purity phenol resin or resin composition obtained by this method has excellent moldability, heat resistance, flame retardancy, etc., and is effective as a sealing resin for electronic components.

In particular, semiconductor devices sealed with the resin composition have excellent heat resistance, moisture resistance, and flame retardance.

[Brief explanation of drawings]

FIG. 1 is a sectional view showing the structure of a planar transistor of the present invention, FIG. 2 is a sectional view showing the structure of a semiconductor device having an integrated circuit, and FIG. 3 is a semiconductor device having a two-layer wiring structure on the surface of a semiconductor substrate. FIG. 4 is a cross-sectional view showing the structure of the device, and FIG. 4 is a cross-sectional perspective view showing the structure of the semiconductor memory element. 1.11,41.71...Silicon semiconductor element substrate, 2,4.2.47...Silicon dioxide film, 3...Base electrode, 4...Emitter electrode, 5,13.74...・Wire, 6, 9...undercoat, 7...tab lead. 8... High purity phenol resin composition, 12... External connection lead terminal, 14.77... Bonding pad. 15...Ceramic package, 43.46...Conductor layer, 44...Aminosilane compound film, 48.49.
...Through hole, 45...Polyimide membrane, 76...
α-ray shielding layer. that's all

Claims (1)

[Claims] 1. An organic solvent is added to a resol type phenol resin obtained by condensing a phenol compound and formaldehyde, and then washed with pure water, and the treated resin is heated at 120°C in an amount ten times the amount The electrical conductivity of the extract heated and extracted with water for over 100 hours is 100μS/
1. A method for producing a high-purity phenol resin, which comprises repeating the washing process until the amount of halogen ions, ammonium ions, or metal ions is 10 ppm or less, pH is 3 to 7, and the amount of halogen ions, ammonium ions, or metal ions is each 10 ppm or less. 2. The number average molecular weight of the resol type phenolic resin is 4.
00 or more, and the amount of unreacted phenol in the resin is 1% by weight or less. 3. The electrical conductivity of the extract obtained by heating and extracting the resol type phenol resin that has been washed with an organic solvent and pure water with 10 times the amount of hot water at 120°C for over 100 hours is 100μS/
A high-purity phenol resin characterized in that it has a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions of 10 ppm or less. 4. The number average molecular weight of the resol type phenolic resin is 4.
4. The high-purity phenol resin according to claim 3, wherein the unreacted phenol in the resin is 1% by weight or less. 5. The resol type phenolic resin has the following general formula [I
], and 10 times the amount of the resin.
The extract extracted by heating with hot water at 20°C for 100 hours or more has an electrical conductivity of 100 μS/cm or less, a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions each of 10 ppm or less. High purity phenolic resin. ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼ [I] [In the formula, R_1 is H, -CH_2OH or ▲ There are mathematical formulas, chemical formulas, tables, etc. ▼
OH), R_2 is -CH_2- or -CH_2-O-
CH_2-, provided that at least -CH_2-O-
Contains CH_2-. n represents a number from 3 to 10. ] 6. A resol-type phenol resin obtained by condensing a phenol compound and formaldehyde, and 25
An organic solvent was added to a resin composition containing ~5% by weight of epoxy resin, followed by washing treatment with pure water, and the treated resin was heated and extracted with 10 times the amount of hot water at 120°C for over 100 hours. The electrical conductivity of the extract is 100μS/
cm or less, pH is 3 to 7, and the cleaning treatment is repeated until the amount of halogen ion, ammonium ion, or metal ion is each 10 ppm or less to remove the organic solvent and water. How to make things. 7. The resol type phenolic resin has the above general formula [I]
The resin has the structure shown in 12
The extract extracted by heating with hot water at 0°C for 100 hours or more has an electrical conductivity of 100 μS/cm or less, a pH of 3 to 7, and an amount of halogen ions, ammonium ions, or metal ions each of 10 ppm or less. 7. The method for producing a resin composition according to claim 6, wherein the resin composition is a high-purity phenolic resin. 8. Extraction in which a resol-type phenolic resin composition containing 25 to 5% by weight of epoxy resin, which has been washed with an organic solvent and pure water, is heated and extracted with 10 times the amount of hot water at 120°C for 100 hours or more. The electrical conductivity of the liquid is 100μS/cm
Hereinafter, a high purity phenol resin composition characterized by having a pH of 3 to 7 and an amount of halogen ion, ammonium ion or metal ion of 10 ppm or less. 9. The resol type phenolic resin has the above general formula [I]
9. The resin composition according to claim 8, having a structure represented by: 10. An electronic device sealed with the resin or resin composition according to any one of claims 3, 4, 5, 8, and 9. 11. A semiconductor device sealed with the resin or resin composition according to any one of claims 3, 4, 5, 8, and 9.