JPH01111408A - Production of glass fiber module - Google Patents

Abstract

PURPOSE:To prevent an adhesive component from being eluted even when a glass fiber module is brought into contact with strong acid and to prevent it from being allowed to come untied by sticking a silane coupling agent or a titanium coupling agent to glass fibers and thereafter interposing thermally- melting fluoroplastic between glass fibers and heating them and thereafter slowly cooling them. CONSTITUTION:Glass fibers are stuck with a primer selected from a silane coupling agent or a titanium coupling agent by immersing glass fibers in the soln. of the primer and thereafter air-drying them. Then thermally-melting fluoroplastic is interposed between the glass fibers by winding sheetlike thermally-melting fluoroplastic thereon and these are heated at the temp. not lower than m.p. of thermally-melting fluoroplastic and thereafter slowly cooled down to about room temp. By such a way, a glass fiber module in which respective glass fibers are joined by the thermally-melting fluoroplastic is obtained.

Description

[Detailed Description of the Invention] The present invention relates to a method for manufacturing a glass fiber module, and more specifically, the present invention relates to a method for manufacturing a glass fiber module.
The present invention relates to a method for manufacturing a glass fiber module that prevents adhesive components from leaking into strong acids or bonded glass fibers from unbundling and falling apart.

Technical aspects of the invention and its problems In recent years, the degree of integration of semiconductors has rapidly progressed, and it has become necessary to form extremely fine patterns on wafers such as silicon. For this reason, it is necessary to prevent fine dust from adhering to wafers such as silicon.

To avoid the adhesion of fine dust on wafers such as silicon, it is necessary to remove fine dust present in the water used to clean the wafer or in the chemicals such as strong acids used in the etching process. is required. In order to remove fine dust present in chemicals such as water or strong acids, water or chemicals such as strong acids are passed through a glass fiber module made by bonding glass fibers. A method that traps fine dust in a glass fiber module may be adopted.

Glass fiber modules made by bonding such glass fibers do not cause any problems when removing dust contained in water, but they do not pose any problems when removing dust contained in strong acids such as concentrated sulfuric acid. In some cases, silicone-based adhesives used as bonding agents for glass fiber modules may leak into strong acids, contaminating the strong acids, or the adhesives may be attacked by strong acids, causing the glass fiber modules to unbundle. There is a short problem.

Purpose of the Invention The present invention aims to solve the above-mentioned problems, and the purpose of the present invention is to solve the above-mentioned problems by preventing adhesive components from dissolving in the strong acid and flowing out even when it comes into contact with a strong acid such as concentrated sulfuric acid. , and what about glass fiber modules that will not cause the bonded glass fiber modules to unbundle and fall apart? ! The purpose is to provide a method for creating

Summary of the Invention The method for manufacturing a glass fiber module according to the present invention includes attaching at least one primer selected from a silane coupling agent or a titanium coupling agent to glass fibers, and then applying a heat-melting fluororesin between the glass fibers. The method is characterized in that the glass fibers are joined by heating the thermofusible fluororesin to a temperature higher than its melting point, and then slowly cooling it.

In the method for manufacturing a glass fiber module according to the present invention, after attaching at least one kind of primer selected from a silane coupling agent or a titanium coupling agent to glass fibers, a heat-melting fluororesin is interposed between the glass fibers. Since the glass fibers are joined by heating to a temperature above the melting point of this hot-melt fluororesin and then slowly cooling it, the fluororesin used as an adhesive will not be attacked even if it comes into contact with strong acids such as concentrated sulfuric acid. Therefore, the strong acid will not be contaminated or the glass fiber module will not unbundle and fall apart. Therefore, the glass fiber module manufactured by the present invention can remove fine dust contained in the strong acid. It can be used when

DETAILED DESCRIPTION OF THE INVENTION The method for manufacturing a glass fiber module according to the present invention will be specifically described below.

In the present invention, a glass fiber module is manufactured by joining a plurality of glass fibers, and the glass fibers may be made of quartz glass, soda lime glass, borosilicate glass, aluminosilicate glass, aluminoborosilicate glass, etc. Although it may be made of glass, it is preferably made of heat-resistant glass such as borosilicate glass.

The fiber diameter of such glass fiber is 50 μ to 3 m.
The thickness is preferably about 300 to 500 μm.

In the present invention, first, at least one kind of plasmar selected from a silane coupling agent or a titanium coupling agent is coated on the glass fiber as described above.

Specifically, the following compounds are used as the silane coupling agent used in the present invention.

1) N112C112Cl12 NtlCt12Cl
12 CH2S! (OCH3> 32) NH2CH2
CH2N11CH2CH2CH2S! (OCH3>3
Oligomer 3) NHCH2CH2CH2ClI23i (OCH3
> 34) NH2Cl12 CH2CH2S! (O
C2115>3go5) NH5t(OCH3)3 etc.

Further, as the titanium coupling agent, specifically, the following compounds are used.

1) [(Cll) CtlO] T+[0P
(0)(OH)OP(0)(OCa'17)2]2 2)OCH2C00Ti[0P(0)(Otl)OP(
0) (QCs 1117) 22 etc.

The silane coupling agent or titanium coupling agent as described above may be used alone or in combination.

In the present invention, a thermofusible fluororesin is interposed between the glass fibers to which such a primer is attached.

Examples of heat-melting fluororesins include copolymers of tetrafluoroethylene and hexafluoropropylene (FEP), copolymers of tetrafluoroethylene and perfluoroalkyl vinyl ether (PFA), and copolymers of tetrafluoroethylene and ethylene. copolymers with , trifluorochloroethylene resins, vinylidene fluoride resins, tetrafluoroethylene resins, etc. are used.

Among these, FEP, PFA, trifluorochloroethylene resin, or tetrafluoroethylene resin as described above is preferably used.

These heat-melting fluororesins are interposed between glass fibers in the form of a sheet or film. In order to interpose a sheet or film of thermofusible fluororesin between glass fibers, a sheet or film of thermofusible fluororesin may be wrapped around the outer periphery of each glass fiber. A fluororesin may be melted and glass fibers may be immersed in the molten fluororesin to provide a film or sheet of heat-melting fluororesin between the glass fibers.

The heat-melting fluororesin thus interposed between the glass fibers is then heated to a temperature equal to or higher than the melting point of the heat-melting fluororesin in, for example, an electric furnace. The heating temperature at this time is determined from the melting point of each heat-melting fluororesin.
Preferably, the temperature is 20 to 80°C higher. Heating at a temperature exceeding 80"C above the melting point is not preferable because the fluororesin may deteriorate due to decomposition or the like.
'Specifically, when using a copolymer of tetrafluoroethylene and hexafluoropropylene (FEP), 330 to 3
It is preferable to heat to 80'C, and when a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether (PFA) is used, it is preferable to heat to 330 to 370C. When trifluorochloride ethylene resin is used for the coating, it is preferably heated to 260 to 280°C, and when a copolymer of tetrafluoroethylene and ethylene is used, it is heated to 300 to 330°C. It is preferable. When vinylidene fluoride resin is used, it is preferable to heat to 200 to 280'C, and when tetrafluoroethylene resin is used, it is preferably heated to 370 to 380'C.
Preferably, heating to .degree.

The heating time varies greatly depending on the heating temperature, but is usually about 10 minutes to 2 hours, preferably about 15 minutes to 1 hour.

After heating the glass fibers with a heat-melting fluororesin interposed between them as described above above the melting point of the heat-melting fluororesin, it is slowly cooled in an electric furnace or the like. The speed is 0.7-30'C/min, preferably 2-30'C/min.
b is desirable.

When the glass fibers are slowly cooled to near room temperature in this manner, a glass fiber module in which each glass fiber is bonded with a thermofusible fluororesin is obtained.

In this glass fiber module, each glass fiber is firmly bonded with heat-melting fluororesin, and this heat-melting fluororesin has excellent chemical resistance against chemicals such as strong acids such as concentrated sulfuric acid. Because it has properties, it will not be attacked even if it comes into contact with chemicals such as strong acids.

Therefore, impurities will not dissolve in chemicals such as strong acids and will not flow out, and furthermore, the glass fiber module will not unbundle and fall apart. Therefore, the glass fiber module manufactured according to the present invention can be used to remove fine dust contained in chemicals such as strong acids.

On the other hand, a glass fiber module made by bonding individual glass fibers with a silicone adhesive can be used to remove fine dust contained in water, etc., but it can be used to remove fine dust contained in water etc. When used to remove fine dust contained therein, the strong acid attacks the silicone adhesive, contaminates the strong acid, and causes the glass fiber module to unbundle and fall apart.

Further, when comparing the adhesion strength between the glass fibers, the glass fibers bonded according to the present invention are bonded as strongly as the glass fibers bonded using a silicon adhesive.

Effects of the Invention In the method for manufacturing a glass fiber module according to the present invention, after attaching at least one type of primer selected from a silane coupling agent or a titanium coupling agent to glass fibers, a thermofusible fluororesin is applied between the glass fibers. Since the glass fibers are bonded by heating to a temperature above the melting point of the hot-melt fluororesin and then gradually cooling it, the fluororesin as an adhesive can be used even if it comes into contact with strong acids such as concentrated sulfuric acid. Therefore, the strong acid will not be contaminated or the glass fiber module will not unbundle and fall apart. It can be used to remove dust.

Example 1 Oligomer of γ-(2-aminoethyl)aminopropyltrimethoxysilane [Toshi Silicon Product No. 52605
0] A glass fiber having an outer diameter of 100 μm was immersed for 5 minutes in a mixed solution consisting of a 3-layer matrix, a methanol 97-type assembly, and a 10-layer assembly of water, and then taken out and air-dried. Next, after heat-treating the air-dried glass fibers at a temperature of 130°C for 30 minutes, three glass fibers were bundled, and an FEP film with a thickness of 11nIr1 and a width of 1.5M was wrapped around the ends, and two sets of these glass fiber bundles were , FEP film wrapping C part was overlapped and fixed.

Two sets of glass fiber bundles fixed in this way were heated to a temperature of 3
The glass fiber bundles were heated for 20 minutes in an electric furnace at 50° C. to fuse the glass fiber bundles, and then slowly cooled to room temperature in the electric furnace to join the two sets of glass fiber bundles.

The bonded glass fiber bundles were immersed in concentrated sulfuric acid at 130'C for 9 days, washed with water, and then subjected to a tensile test using a tensile tester (Autograph).

The results are shown in Table 1.

Example 2 Two sets of glass fiber bundles were joined together and a tensile test was conducted in the same manner as in Example 1, except that a PFA film was used instead of the FEP film.

The results are shown in Table 1.

In Example 1, 3 parts by weight of γ-(2-aminoethyl)aminopropyltrimethoxysilane oligomer [Toshi Silicon N product number 5Z6050] and 97 parts by weight of methanol.
[
(He)2CHO]2Ti[0P(0)(OH)O
A compound having the structural formula of P(0)(QC8H1□)2]2 [manufactured by Ajinomoto ■, product number 338X] Except for using a mixed solution consisting of 1 double part and 100ffiffi parts of isopropyl alcohol (IPA). In the same manner as in Example 1, two sets of glass fiber bundles were joined and a tensile test was conducted.

The results are shown in Table 1.

Example 4 Two sets of glass fiber bundles were joined together and subjected to a tensile test in the same manner as in Example 3, except that a PFA film was used instead of the FEP film.

The results are shown in Table 1.

In Example 1, 3 parts by weight of γ-(2-aminoethyl)aminopropyltrimethoxysilane oligomer [Toshi Silicon Fit product number 5Z6050], 97 parts by weight of methanol, and 10 parts by weight of water were used. OCH2COOTi[0P(0)(OH)OP(0)
Same as Example 1 except that a mixed solution consisting of 1 part by weight of a compound having the structural formula of (QC8H1□)212 [manufactured by Ajinomoto <+a, product number KR138S] and 100 parts by weight of isopropyl alcohol (IPA) was used. Two sets of glass fiber bundles were bonded together and a tensile test was conducted.

The results are shown in Table 1.

Example 6 Two sets of glass fiber bundles were joined together and a tensile test was conducted in the same manner as in Example 5, except that a PFA film was used instead of the FEP film.

The results are shown in Table 1.

Comparative Example 1 Three glass fibers with an outer diameter of 100μ are bundled, and a silicone resin film with a thickness of 11run and a width of 1.5# is wrapped around the end of the bundle, and then two sets of these glass fiber bundles are wrapped with a silicone resin film. The parts were overlapped and fixed.

Two sets of glass fiber bundles fixed in this way were heated to a temperature of 3
One set of glass fiber bundles was fused by heating in an electric furnace at 50'C for 20 minutes, and two sets of glass fiber bundles were joined by slowly cooling to room temperature in an electric furnace.

The bonded glass fiber bundles were immersed in concentrated sulfuric acid at 130'C for 9 days, washed with water, and then subjected to a tensile test using a tensile tester (Autograph).

The results are shown in Table 1.

Claims (1)

[Claims] After attaching at least one type of primer selected from a silane coupling agent or a titanium coupling agent to glass fibers, a heat-melting fluororesin is interposed between the glass fibers, and the temperature is higher than the melting point of the heat-melting fluororesin. 1. A method for manufacturing a glass fiber module, which comprises heating the glass fibers to a temperature of 100.degree. C., followed by slow cooling to join the glass fibers.