USH836H - Method for analysis of finishing agent applied to glass fiber substrate - Google Patents
Method for analysis of finishing agent applied to glass fiber substrate Download PDFInfo
- Publication number
- USH836H USH836H US07/210,664 US21066488A USH836H US H836 H USH836 H US H836H US 21066488 A US21066488 A US 21066488A US H836 H USH836 H US H836H
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- US
- United States
- Prior art keywords
- glass fiber
- fiber substrate
- finishing agent
- analysis
- infrared
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 30
- 239000000758 substrate Substances 0.000 title claims abstract description 25
- 238000004458 analytical method Methods 0.000 title claims description 11
- 238000010521 absorption reaction Methods 0.000 claims abstract description 20
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 15
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 12
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims abstract description 8
- 230000001678 irradiating effect Effects 0.000 claims abstract 2
- DGJPPCSCQOIWCP-UHFFFAOYSA-N cadmium mercury Chemical compound [Cd].[Hg] DGJPPCSCQOIWCP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052714 tellurium Inorganic materials 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 claims description 3
- 108010067216 glycyl-glycyl-glycine Proteins 0.000 claims 1
- GZXOHHPYODFEGO-UHFFFAOYSA-N triglycine sulfate Chemical compound NCC(O)=O.NCC(O)=O.NCC(O)=O.OS(O)(=O)=O GZXOHHPYODFEGO-UHFFFAOYSA-N 0.000 claims 1
- 238000000862 absorption spectrum Methods 0.000 description 8
- 239000002759 woven fabric Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 238000011088 calibration curve Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000275 quality assurance Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 description 1
- 101100386054 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) CYS3 gene Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 101150035983 str1 gene Proteins 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- PGAPATLGJSQQBU-UHFFFAOYSA-M thallium(i) bromide Chemical compound [Tl]Br PGAPATLGJSQQBU-UHFFFAOYSA-M 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Definitions
- the present invention relates to a method for rapid and accurate qualitative and quantitative analysis of a finishing agent applied to the surface of a glass fiber substrate.
- Printed wiring board are necessarily dipped in a molten solder bath during production of the printed wiring board and a significant problem is separation of glass cloth and epoxy resin at their interface due to thermal shock at the dipping.
- the present invention provides a method for accurate and rapid qualitative and quantitative analysis of finishing agents such as coupling agent, surface active agent and the like applied to the surface of a glass fiber substrate for printed wiring board.
- FIG. 1 shows an infrared absorption spectrum of a glass fiber woven fabric treated with epoxy silane of 0.6% by weight in concentration.
- FIG. 2 is a calibration curve which shows the relation between concentration of epoxy silane and absorption peak intensity of 2940 cm -1 .
- FIG. 3 is a calibration curve which shows the relation between concentration and deposition rate of epoxy silane according to the ignition of loss method.
- FIG. 4 is a disassembling side view of a partial cross section of a sample holder.
- FIG. 5 is an infrared absorption spectrum of a glass fiber woven fabric treated with aminosilane of 0.6% by weight in concentration.
- FIG. 6 is a calibration curve which shows the relation between concentration of aminosilane and absorption peak intensity of 2933 cm -1 .
- the present invention is a method for analysis of a finishing agent on glass fiber substrate, characterized in that the glass fiber substrate to be tested is placed in a Fourier transform infrared spectrophotometer equipped with a diffuse reflectance measuring device, said glass fiber substrate is irradiated with infrared rays and qualitative analysis of the finishing agent on the surface of the glass fiber substrate is carried out from wave number of infrared absorption peak produced at the time of the irradiation and quantitative analysis of the finishing agent is carried out from the intensity of the infrared absorption peak.
- a glass fiber substrate applied with a finishing agent used for cloth, woven fabric, non-woven fabric, mat, paper or chopped strand is irradiated with infrared rays from a Fourier transform infrared spectrophotometer and reflected infrared rays are collected by a diffuse reflectance measuring device. Taking the ratio of incident infrared rays and reflected infrared rays at this time, absorption of specific wavelength depending on the structure of the finishing agent can be observed and furthermore, the infrared absorption spectrum obtained at this time is subjected to automatical wave treatment by a computer to display it in a graph.
- the glass fiber substrate shows very strong absorption and anomalous scattering by siloxane bond (Si-O-Si), absorption by the finishing agent cannot be detected in the region of wave number of 1600-1000 cm -1 . Therefore, in order to detect the absorption by organic functional group of finishing agent, it is necessary to measure absorption spectrum in the region of wave number of 3300-2500 cm -1 .
- a Fourier transform infrared spectrophotometer and a diffuse reflectance measuring device with a trialycine sulfate TGS detector or mercury cadmium tellurium MCT detector and a computer with wave separating program.
- a high sensitivity MCT detector is preferred for improvement of accuracy.
- a sample holder According to this sample holder, a sample is put on a sample carrier, a crystal plate of an infrared ray transmitting substance is put on the sample and these are fixed by a fastener from above.
- sample carrier As the crystal plates of infrared transmitting substance provided on sample carrier, there may be preferably used those of ZnSe, Si, KBr, Ge, KRS-5 and the like.
- sample carrier and fastener made of metals which do not affect the wave number of 3300-2500 cm -1 and stainless steel is especially preferred.
- Any wave form separating programs may be conveniently used as far as they can separate overlapping two or more infrared absorption peaks.
- the method of the present invention makes it possible to perform non-destructive analysis of a glass fiber substrate. Furthermore, according to the method of the present invention, qualitative and quantitative analysis becomes possible from the position, and height or area of the peak of the infrared absorption spectrum. With reference to the necessary amount of sample, several ten grams is required in the case of the conventional ignition of loss method while only several milligrams is sufficient for the analytical method of the present invention. Further, the conventional ignition loss method requires 3 hours for measurement while measurement can be completed in only in 10 minutes according to the method of the present invention. Thus the, necessary amount of material and time required for measurement can be greatly reduced.
- a heat treated and degreased glass fiber woven fabric (Tradename: WEA-18W manufactured by Nitto Boseki Co., Ltd.) of 212 g/m 2 in unit weight was used as a glass fiber substrate.
- silane coupling agent (Tradename: EPOXYSILANE A-187 for ⁇ -gIycidoxypropyltrimethoxysilane manufactured by Japan Uniker Co.) of 0.2%, 0.4%, 0.6%, 0.8%, 1.0%, 1.2% and 1.4% in concentration were adjusted to pH 4 with acetic acid. These were used as finishing agents.
- the above woven fabric was dipped in each of these solutions, then squeezed to pick-up 25% by mangle and thereafter dried by heating at 110° C. for 30 minutes.
- sample holder 1 made of stainless steel as shown in FIG. 4 on a of diffuse reflectance measuring device of Fourier transform infrared spectrophotometer system [JIR-3510 manufactured by Nippon Denshi Co. including high sensitivity MCT detector IR-DET 101, diffuse reflectance measuring device IR-DRA 110 and wave form separating program (Lorentjian and Gaussian curve fitting)].
- the sample holder 1 comprises a sample carrier 2 made of stainless steel, an infrared transmitting crystal plate 3 which is put on the sample carrier and a stainless steel fastener 4.
- the sample was put on the sample carrier 2 and covered with infrared transmitting crystal plate 3 (crystal plate of KBr in this example). These were further covered with stainless steel fastener 4, thereby to firmly fix the sample.
- This holder with the sample which was uniformly stretched to remove shrinkage of glass fiber woven fabric was inserted in the diffuse reflectance measuring device and was irradiated with infrared ray and the infrared absorption spectrum was measured.
- FIG. 1 shows an infrared spectrum of the sample treated with 0.6% aqueous solution of epoxysilane.
- the peaks at 3055 cm -1 and 2990 cm -1 in FIG. 1 show stretching vibration of C-H of epoxy group ##STR1## and clearly show presence of epoxysilane. That is, this means
- the absorption peak at 2940 cm -1 shows stretching vibration of C--H of CH 2 and quantitative analysis can be performed from calibration curve prepared by measuring height or area of the peak.
- FIG. 2 is a graph which shows the relation between concentration of the epoxysilane and intensity of infrared absorption peak at 2940 cm -1 .
- epoxysilane concentration is low, it may be considered that selective adsorption of epoxysilane does not occur and thus it can be considered that the epoxysilane concentration is in proportion to deposition amount onto glass fiber substrate. Therefore, FIG. 2 can be said to show relation between the deposition amount and peak intensity.
- FIG. 3 is a graph which shows the relation between epoxysilane concentration and deposition amount measured by the conventional ignition of loss method.
- FIG. 2 is far less in scattering than FIG. 3 and superior to FIG. 3 in linearity and thus the method of the present invention is high in reliability as a method of quantitative analysis.
- Example 1 The procedure of Example 1 was repeated except that a silane coupling agent (Tradename: KBM-573, N-phenyl- ⁇ -aminopropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.) was used in place of epoxysilane and infrared absorption spectrum was measured.
- a silane coupling agent (Tradename: KBM-573, N-phenyl- ⁇ -aminopropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.) was used in place of epoxysilane and infrared absorption spectrum was measured.
- FIG. 5 shows an infrared absorption spectrum of the sample treated with a 0.6% aqueous solution of N-phenyl- ⁇ -aminopropyltrimethoxysilane.
- the absorption peak at 3410 cm -1 in FIG. 1 shows stretching vibration of amino group (NH) and absorption peaks at 3084, 3050 and 3020 cm -1 indicate stretching vibrations of C--H of benzene ring.
- the absorption peak at 2933 cm -1 indicates stretching vibration of C--H of CH 2 and quantitative analysis can be performed from a calibration curve prepared by measuring the height or area of this peak.
- FIG. 6 shows the relation between the aminosilane concentration and intensity of the infrared absorption peak at 2933 cm -1 . It can be seen therefrom that a superior linear relation can be obtained between the concentration and the peak intensity.
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Disclosed is a method for rapid and accurate qualitative and quantitative analysis of finishing agent applied onto the surface of a glass fiber substrate. This method comprises placing a glass fiber substrate to be tested in a Fourier transform infrared spectrophotometer equipped with a diffuse reflectance measuring device, irradiating said glass fiber substrate with infrared ray and carrying out qualitative analysis of finishing agent on the surface of the glass fiber substrate from wave number of infrared absorption peak produced at the irradiation and quantitative analysis of the finishing agent from intensity of the infrared absorption peak.
Description
The present invention relates to a method for rapid and accurate qualitative and quantitative analysis of a finishing agent applied to the surface of a glass fiber substrate.
Hitherto, as a method for qualitative and quantitative analysis of finishing agent on glass fiber substrate for printed wiring boards, there has been known "New Qualitative and Quantitative Analytical Method for Coupling Agent on Glass Cloth" Preprint Section 18-A (1961) of The Society of the Plastics Industry, Inc. This method utilizes color reaction of indicators (Methylene Blue method, Bromocresol Green method, etc.). In Japan, ignition of loss method according to JIS-R-3420 has been widely employed for quantitative analysis.
Printed wiring board are necessarily dipped in a molten solder bath during production of the printed wiring board and a significant problem is separation of glass cloth and epoxy resin at their interface due to thermal shock at the dipping.
This interfacial separation is greatly affected by properties of the finishing agent for glass fiber substrate. Therefore specifying the kind of the finishing agent and weighing thereof must be carried out accurately and rapidly.
Analysis of a the finishing agent applied to the surface of glass fiber substrate which greatly affects the performances of printed wiring board has been conducted by ignition of loss method which comprises heating a sample to 625° C. to burn the finishing agent which is an organic material.
However, this ignition of loss method has the following defects: (1) Qualitative analysis of finishing agent is impossible; (2) Measurement requires very long time; (3) Accuracy of quantitative analysis is not high.
Quality assurance of printed wiring board by the ignition of loss method cannot sufficiently express the state of finishing agent and besides rapid measure is impossible because of long time required for measurement.
Analysis of a finishing agent applied onto the surface of a glass fiber substrate by infrared absorption method is also attempted. (See, for example, "Sen-i Gakkaishi" vol. 43 (1987) page 313 and "Applied Spectroscopy", vol. 38 (1984), page 1). However, according to such a method, when the amount of finishing agent contained in the sample is small and especially when the deposition amount of finishing agent is small because the surface area is small as in industrial products which are relatively large in fiber diameter the, spectrum is indefinite and the analysis is difficult.
The present invention provides a method for accurate and rapid qualitative and quantitative analysis of finishing agents such as coupling agent, surface active agent and the like applied to the surface of a glass fiber substrate for printed wiring board.
FIG. 1 shows an infrared absorption spectrum of a glass fiber woven fabric treated with epoxy silane of 0.6% by weight in concentration.
FIG. 2 is a calibration curve which shows the relation between concentration of epoxy silane and absorption peak intensity of 2940 cm-1.
FIG. 3 is a calibration curve which shows the relation between concentration and deposition rate of epoxy silane according to the ignition of loss method.
FIG. 4 is a disassembling side view of a partial cross section of a sample holder.
FIG. 5 is an infrared absorption spectrum of a glass fiber woven fabric treated with aminosilane of 0.6% by weight in concentration.
FIG. 6 is a calibration curve which shows the relation between concentration of aminosilane and absorption peak intensity of 2933 cm-1.
The present invention is a method for analysis of a finishing agent on glass fiber substrate, characterized in that the glass fiber substrate to be tested is placed in a Fourier transform infrared spectrophotometer equipped with a diffuse reflectance measuring device, said glass fiber substrate is irradiated with infrared rays and qualitative analysis of the finishing agent on the surface of the glass fiber substrate is carried out from wave number of infrared absorption peak produced at the time of the irradiation and quantitative analysis of the finishing agent is carried out from the intensity of the infrared absorption peak.
According to the present invention, a glass fiber substrate applied with a finishing agent used for cloth, woven fabric, non-woven fabric, mat, paper or chopped strand is irradiated with infrared rays from a Fourier transform infrared spectrophotometer and reflected infrared rays are collected by a diffuse reflectance measuring device. Taking the ratio of incident infrared rays and reflected infrared rays at this time, absorption of specific wavelength depending on the structure of the finishing agent can be observed and furthermore, the infrared absorption spectrum obtained at this time is subjected to automatical wave treatment by a computer to display it in a graph.
Since the glass fiber substrate shows very strong absorption and anomalous scattering by siloxane bond (Si-O-Si), absorption by the finishing agent cannot be detected in the region of wave number of 1600-1000 cm-1. Therefore, in order to detect the absorption by organic functional group of finishing agent, it is necessary to measure absorption spectrum in the region of wave number of 3300-2500 cm-1.
In order to perform accurate and rapid analysis, usually measurement is carried out by the combination of a Fourier transform infrared spectrophotometer and a diffuse reflectance measuring device with a trialycine sulfate TGS detector or mercury cadmium tellurium MCT detector and a computer with wave separating program. In this case, use of a high sensitivity MCT detector is preferred for improvement of accuracy. It is similarly preferred to use a sample holder. According to this sample holder, a sample is put on a sample carrier, a crystal plate of an infrared ray transmitting substance is put on the sample and these are fixed by a fastener from above.
As the crystal plates of infrared transmitting substance provided on sample carrier, there may be preferably used those of ZnSe, Si, KBr, Ge, KRS-5 and the like. When the sample holder is used, it is preferred to use the sample carrier and fastener made of metals which do not affect the wave number of 3300-2500 cm-1 and stainless steel is especially preferred.
Any wave form separating programs may be conveniently used as far as they can separate overlapping two or more infrared absorption peaks.
Being different from the conventional ignition of loss method, the method of the present invention makes it possible to perform non-destructive analysis of a glass fiber substrate. Furthermore, according to the method of the present invention, qualitative and quantitative analysis becomes possible from the position, and height or area of the peak of the infrared absorption spectrum. With reference to the necessary amount of sample, several ten grams is required in the case of the conventional ignition of loss method while only several milligrams is sufficient for the analytical method of the present invention. Further, the conventional ignition loss method requires 3 hours for measurement while measurement can be completed in only in 10 minutes according to the method of the present invention. Thus the, necessary amount of material and time required for measurement can be greatly reduced.
The following nonlimiting examples illustrate preferred embodiments of the analytical method of the present invention. All % in the examples mean % by weight.
A heat treated and degreased glass fiber woven fabric (Tradename: WEA-18W manufactured by Nitto Boseki Co., Ltd.) of 212 g/m2 in unit weight was used as a glass fiber substrate.
Aqueous solutions of silane coupling agent (Tradename: EPOXYSILANE A-187 for γ-gIycidoxypropyltrimethoxysilane manufactured by Japan Uniker Co.) of 0.2%, 0.4%, 0.6%, 0.8%, 1.0%, 1.2% and 1.4% in concentration were adjusted to pH 4 with acetic acid. These were used as finishing agents.
The above woven fabric was dipped in each of these solutions, then squeezed to pick-up 25% by mangle and thereafter dried by heating at 110° C. for 30 minutes.
A circular sample of 10 mm in diameter was cut out from said glass fiber woven fabric applied with the finishing agent. This sample was fixed by sample holder 1 made of stainless steel as shown in FIG. 4 on a of diffuse reflectance measuring device of Fourier transform infrared spectrophotometer system [JIR-3510 manufactured by Nippon Denshi Co. including high sensitivity MCT detector IR-DET 101, diffuse reflectance measuring device IR-DRA 110 and wave form separating program (Lorentjian and Gaussian curve fitting)]. The sample holder 1 comprises a sample carrier 2 made of stainless steel, an infrared transmitting crystal plate 3 which is put on the sample carrier and a stainless steel fastener 4. The sample was put on the sample carrier 2 and covered with infrared transmitting crystal plate 3 (crystal plate of KBr in this example). These were further covered with stainless steel fastener 4, thereby to firmly fix the sample. This holder with the sample which was uniformly stretched to remove shrinkage of glass fiber woven fabric was inserted in the diffuse reflectance measuring device and was irradiated with infrared ray and the infrared absorption spectrum was measured.
FIG. 1 shows an infrared spectrum of the sample treated with 0.6% aqueous solution of epoxysilane. The peaks at 3055 cm-1 and 2990 cm-1 in FIG. 1 show stretching vibration of C-H of epoxy group ##STR1## and clearly show presence of epoxysilane. That is, this means
that qualitative analysis can be performed.
The absorption peak at 2940 cm-1 shows stretching vibration of C--H of CH2 and quantitative analysis can be performed from calibration curve prepared by measuring height or area of the peak.
FIG. 2 is a graph which shows the relation between concentration of the epoxysilane and intensity of infrared absorption peak at 2940 cm-1. When epoxysilane concentration is low, it may be considered that selective adsorption of epoxysilane does not occur and thus it can be considered that the epoxysilane concentration is in proportion to deposition amount onto glass fiber substrate. Therefore, FIG. 2 can be said to show relation between the deposition amount and peak intensity.
FIG. 3 is a graph which shows the relation between epoxysilane concentration and deposition amount measured by the conventional ignition of loss method.
When comparing FIG. 2 and FIG. 3, it can be seen that FIG. 2 is far less in scattering than FIG. 3 and superior to FIG. 3 in linearity and thus the method of the present invention is high in reliability as a method of quantitative analysis.
The procedure of Example 1 was repeated except that a silane coupling agent (Tradename: KBM-573, N-phenyl-γ-aminopropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.) was used in place of epoxysilane and infrared absorption spectrum was measured.
FIG. 5 shows an infrared absorption spectrum of the sample treated with a 0.6% aqueous solution of N-phenyl-γ-aminopropyltrimethoxysilane. The absorption peak at 3410 cm-1 in FIG. 1 shows stretching vibration of amino group (NH) and absorption peaks at 3084, 3050 and 3020 cm-1 indicate stretching vibrations of C--H of benzene ring. These results clearly show the presence of N-phenyl-Y-aminopropyltrimethoxysilane.
Further, the absorption peak at 2933 cm-1 indicates stretching vibration of C--H of CH2 and quantitative analysis can be performed from a calibration curve prepared by measuring the height or area of this peak.
FIG. 6 shows the relation between the aminosilane concentration and intensity of the infrared absorption peak at 2933 cm-1. It can be seen therefrom that a superior linear relation can be obtained between the concentration and the peak intensity.
As explained above, qualitative analysis and quantitative analysis of a finishing agent applied to a glass fiber substrate for printed wiring board can be highly accurately and rapidly carried out by the analytical method of the present invention which utilizes a Fourier transform infrared spectrophotometer. Therefore, the method can be applied to quality assurance of printed wiring boards which depend on finishing agents and thus makes a great contribution to increase reliability of quality and dissolution of problems in interfaces of glass fiber reinforced composite materials.
Claims (3)
1. A method for analysis of a finishing agent applied to a glass fiber substrate which comprises placing a glass fiber substrate to be tested in a Fourier transform infrared spectrophotometer equipped with a diffuse reflectance measuring device, irradiating said glass fiber substrate with an infrared ray and carrying out qualitative analysis of the finishing agent on the surface of the glass fiber substrate from the wave number of an infrared absorption peak produced at the irradiation and quantitative analysis of the finishing agent from the intensity of the infrared absorption peak.
2. A method according to claim 1 wherein the Fourier transform infrared spectrophotometer includes a triglycine sulfate detector or a mercury cadmium tellurium detector and a wave separating program.
3. A method according to claim 2 wherein the mercury cadmium tellurium detector is a high sensitivity mercury cadmium tellurium detector.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP62-185159 | 1987-07-24 | ||
JP18515987A JPS6429740A (en) | 1987-07-24 | 1987-07-24 | Method for analyzing surfactant of glass fiber base material |
Publications (1)
Publication Number | Publication Date |
---|---|
USH836H true USH836H (en) | 1990-11-06 |
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ID=16165867
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US07/210,664 Abandoned USH836H (en) | 1987-07-24 | 1988-06-20 | Method for analysis of finishing agent applied to glass fiber substrate |
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US (1) | USH836H (en) |
JP (1) | JPS6429740A (en) |
Cited By (1)
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Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2777696B1 (en) * | 1998-04-17 | 2000-05-26 | Schneider Electric Ind Sa | DEVICE FOR CONTROLLING THE DISCHARGE AND RELEASE OF AN ENERGY ACCUMULATOR DURING THE EXTRACTION OF A PLUG-IN CIRCUIT BREAKER |
JP5193077B2 (en) * | 2009-01-19 | 2013-05-08 | 株式会社アルバック | Surface-modified substrate analysis method, analysis substrate, surface-modified substrate manufacturing method, and surface-modified substrate |
JP5193078B2 (en) * | 2009-01-19 | 2013-05-08 | 株式会社アルバック | Analysis method and manufacturing method of surface modified substrate |
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1987
- 1987-07-24 JP JP18515987A patent/JPS6429740A/en active Pending
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1988
- 1988-06-20 US US07/210,664 patent/USH836H/en not_active Abandoned
Non-Patent Citations (7)
Title |
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Abstract published in an annual meeting of Kobunski Gakkai, May 1988: 27-H-15. |
Applied Spectroscopy, vol. 38, No. 1, pp. 1-7 (1984) Culler et al. |
News Paper (Nihon Kogyo Shinbun), issued Jun. 22, 1987. |
News Paper (Nikkan Kogyo Shinbun), issued Jun. 22, 1987. |
News Paper (Nitsukei Sangyo Shinbun), issued Jun. 22, 1987. |
Sen-i Gakkaishi, vol. 43, No. 6, pp. 313-319 (1987) Ikuta et al. |
Willey, "FTIR Spectrophotometer for Transmittance and Diffuse Reflectance Measurements" Applied Spectroscopy, vol. 30 (No. 6), 1976, pp. 593-601. |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114088654B (en) * | 2021-10-12 | 2024-06-04 | 南京玻璃纤维研究设计院有限公司 | Method for evaluating effectiveness of glass fiber coating and application thereof |
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JPS6429740A (en) | 1989-01-31 |
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