JPH05208836A - Production of glass thin film and production system therefor - Google Patents

Abstract

PURPOSE:To obtain a glass thin film having a desired composition by respectively detecting the intensities at plural wavelengths of the radiation emitted from each substrate to control the composition of a glass thin film formed on the substrate. CONSTITUTION:Plural substrates 11 are put on turntable 12 at the lower part of a reaction vessel 16. Each of the substrates 11 is e.g. a SiO2 wafer, Si wafer. A glass fine particle layer is formed on each substrate 11 through a flame stream from a burner 13 at the upper part of the reaction vessel 16. The respective outputs from interference-type infrared photometers 19, 119 are analyzed by a CPU 30 to determine concentrations of SiO2, B2O3, P2O5, etc., which are, in turn, used as the information for controlling a heater controller 34, etc. Thereby, the composition of the glass fine particles built up on the substrates 11 can be kept uniform, or brought to a desired distribution.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for manufacturing a glass thin film used for forming an optical waveguide or the like.

[0002]

2. Description of the Related Art FIG. 1 shows an apparatus for carrying out a conventional method for producing an oxide glass thin film. A plurality of substrates 1 are placed on the turntable 2 in the reaction container 6. Glass fine particles are deposited on these substrates 1 along with the flame flow from the torch 3. The glass particles and exhaust gas not deposited on the substrate 1 are sucked into the exhaust pipe 4. In this case, since the glass particles are uniformly deposited on the substrate 1, the turntable 2 on which the substrate 1 is placed is rotated about the central vertical axis. Further, the torch 3 is also reciprocated within the predetermined range in the radial direction of the turntable 2. The turntable 2 is provided with a lower heater 5 to uniformly heat the substrate 1 on the turntable 2. The specific contents of the conventional example are described in detail in JP-A-58-105111.

[0003]

However, in the case of the above-mentioned conventional apparatus, the composition of the glass fine particle layer is determined during the formation of the glass fine particle layer under various conditions such as the feed amount of the raw material / fuel to the torch 3 and the temperature of the turntable 2. However, the composition of the finally obtained oxide glass thin film could not be sufficiently controlled and adjusted.

Therefore, according to the present invention, by increasing the accuracy of measuring the composition of the glass fine particle layer during formation,
An object of the present invention is to provide a method and an apparatus for producing a glass thin film having a desired composition.

[0005]

In order to solve the above problems, in the method for producing a glass thin film according to the present invention, a raw material is supplied together with an oxyhydrogen flame into a reaction vessel to produce glass fine particles, and the glass fine particles are After depositing on the substrate to form a porous thin film, the substrate is heated at a high temperature to make the porous thin film transparent. Furthermore, in such a manufacturing method,
(A) When the porous thin film is formed, the intensities of the emitted light emitted from the substrate at a plurality of wavelengths are detected,
(B) The composition of the porous thin film to be formed on the substrate is controlled by adjusting the conditions for the production of glass particles and the deposition of glass particles according to the intensity ratio of the detected radiated light at the above-mentioned plurality of wavelengths. I am going to do it.

Further, the oxide glass thin film manufacturing apparatus according to the present invention comprises (a) supplying a raw material together with an oxyhydrogen flame into a reaction vessel to generate glass fine particles, and depositing the glass fine particles on a substrate. Flame deposition means for forming a porous thin film, (b) detection means for detecting the intensities of radiated light emitted from the substrate at a plurality of wavelengths when forming the porous thin film, and (c) detection An apparatus for producing a glass thin film, which controls the composition of a porous thin film to be formed on the substrate by adjusting the flame deposition means according to the intensity ratio of the radiated light detected by the means at the plurality of wavelengths.

[0007]

According to the above method for producing an oxide glass thin film, when the porous thin film is formed, the intensities of the radiated light emitted from the substrate at a plurality of wavelengths are detected, and the intensity ratio is determined according to the intensity ratio of these. The composition of the porous thin film to be formed on the substrate is controlled by adjusting the conditions for the production of glass particles and the deposition of glass particles. in this case,
Since the intensity ratio of synchrotron radiation at multiple wavelengths corresponds to the composition ratio of the porous thin film, it is possible to improve the measurement accuracy of the composition during the formation of the porous thin film, and the glass having the desired composition A thin film can be provided.

Further, according to the above oxide glass thin film manufacturing apparatus, when the porous thin film is formed, the detecting means detects the intensity of the radiated light emitted from the substrate at a predetermined wavelength, and the composition controlling means. According to the detection result of the detection means, the flame deposition means is adjusted to control the composition of the porous thin film to be formed on the substrate. For this reason,
The accuracy of measuring the composition of the porous thin film during formation can be improved, and a glass thin film having a desired composition can be provided.

[0009]

EXAMPLES Examples of the present invention will be specifically described below.

FIG. 2 is a perspective view showing the structure of the glass thin film manufacturing apparatus according to the embodiment. A plurality of substrates 11 are placed on a turntable 12 provided below the reaction container 16. As the substrate 11, a SiO ₂ wafer, a Si wafer, or the like can be used. Glass fine particles are supplied onto each substrate 11 along with a flame flow from a burner 13 provided above the reaction vessel 16. As a result, a glass fine particle layer is formed on each substrate 11.
The glass particles and the exhaust gas not deposited on the substrate 11 are sucked into the exhaust pipe 4 provided on the side of the reaction container 16. The infrared window 18 provided on the upper part of the reaction vessel 16 is
The radiated light generated by the substrate 11 is guided to the interferometric infrared photometer 19.

FIG. 3 is a side view of the manufacturing apparatus shown in FIG.
In the turntable 12 provided under the reaction container 16, a heater 12a for keeping the temperature of the substrate 11 constant and improving the adhesion of glass particles to the substrate 11 is fixed. The heater 12a is heated by the power supply 20 provided outside while monitoring the temperature of the turntable 12.

A turntable 1 for supporting the substrate 11 in order to uniformly supply and deposit fine glass particles on the substrate 11.
2 rotates in the horizontal plane. The burner 13 also reciprocates in the radial direction of rotation of the turntable 12. As a result, the burner 13 is two-dimensionally scanned with respect to the turntable 12.

FIG. 4 is a diagram showing a part of a control system of the manufacturing apparatus of FIG. Radiation light generated by the substrate 11 is guided to the interferometric infrared photometer 19. On the other hand, another interferometric infrared photometer 119 is provided with the reference light from the comparative material 111.
It is incident through 18a. Comparative material 111 is a fused quartz substrate heated at a constant temperature. Each of the interferometric infrared photometers 19 and 119 is made up of Si- in the emission intensity distribution of the emitted light or the reference light generated by the substrate 11 or the comparative material 111.
Emission peaks corresponding to lattice vibrations such as O-bonds, B-O bonds, and P-O bonds are detected to detect the wavelength and its intensity.

The CPU 30 includes each interferometric infrared photometer 19,
The output of 119 is analyzed to analyze SiO ₂ , B ₂ O ₃ , P ₂ O ₅
Etc. to determine the concentration. Obtained SiO ₂ , B ₂ O ₃ , P
The concentrations of ₂ O _{5 and the} like are used as information for controlling the raw material supply system 32, the heater controller 34, and the like. Thereby, the composition of the glass fine particle layer deposited on the substrate 11 can be kept uniform, or the composition of the glass fine particle layer can be formed in a desired distribution.

FIG. 5 is a diagram showing an emission spectrum of a SiO ₂ type glass fine particle layer to which B ₂ O ₃ and P ₂ O ₅ are added. In this case, the temperature of the glass fine particle layer is 750.
It was kept at ℃. As shown in the figure, in the infrared radiant light in the wavelength band of 5 to 15 μm generated by the glass fine particle layer, the emission peak at the wave number of 1080 cm ⁻¹ corresponding to the Si—O bond and the P−
An emission peak at a wave number of 1320 cm ⁻¹ corresponding to O-bonding,
There is an emission peak at a wavenumber of 1420 cm ⁻¹ corresponding to the B—O bond. The intensity of each emission peak is SiO ₂ , B ₂ O
_Since it corresponds to the concentrations of ₃ and P ₂ O ₅ , the composition ratio of the glass fine particle layer can be determined by calculating the intensity ratio of such emission peaks.

FIG. 6 is a diagram showing the relationship between the intensity of each emission peak and the concentration of each component. The B concentration and the P concentration show the results of measuring the soot, which is a glass fine particle layer, by ICP (inductively coupled emission plasma analysis). Also, B-O
The emission intensity ratio corresponding to the bond and the P-O bond is Si-
It is based on the emission intensity of O bond. For example, B
In the case of —O bond, the emission intensity ratio is given by (emission intensity of B—O bond / emission intensity of Si—O bond). As is clear from the table, it is found that the emission intensity ratio corresponding to the B—O bond and the P—O bond has a substantially linear relationship with the B concentration and P concentration in the soot that is the glass fine particle layer. If the relationship between the composition of the glass particle layer and its emitted light is accurately obtained in advance by a preliminary experiment, the composition of this glass particle layer is obtained more accurately from the emitted light generated by the glass particle layer deposited on the substrate 11. be able to.

The operation of the glass thin film manufacturing apparatus according to the embodiment will be briefly described below. H ₂ , O on burner 13
Fuel gas such as ₂ , SiCl ₄ , BCl ₃ , PCl ₃ ,
By supplying a raw material gas such as GeCl ₄ to the raw material gas, the raw material gas is decomposed with permeating water to deposit SiO ₂ -based glass fine particles on each substrate 11. At the same time, turntable 1
Since 2 is rotated and the burner 13 is reciprocated, the glass particles from the burner 13 are uniformly deposited on each substrate 11.

In this case, during formation of the glass fine particle layer, C
The PU 30 analyzes the output of each interferometric infrared photometer 19, 119 to monitor the concentration of B ₂ O ₃ , P ₂ O _5, etc.
Further, since the raw material supply system 32, the heater controller 34, etc. are controlled based on the obtained concentrations of B ₂ O ₃ , P ₂ O _5, etc., the composition of the glass fine particle layer deposited on the substrate 11 is controlled. Can be kept uniform.

Thereafter, each substrate 11 is heated to a high temperature in another furnace to make the deposited glass fine particle layer transparent and obtain a glass thin film. Further, if the composition control is performed in two steps in the above operation, the glass thin film having a high refractive index can be formed on the glass thin film having a low refractive index. An optical waveguide can be formed on each substrate 11 by subjecting this to a lithography technique and etching by RIE or the like to form a glass thin film having a low refractive index thereon.

The present invention is not limited to the above embodiment. For example, without using the comparative material 111, the emission intensity ratio of each emission peak in the emission spectrum of the comparative material 111 is stored in the CPU 30 in advance, and the composition of the glass fine particle layer deposited on the substrate 11 is obtained. You can also

[0021]

As described above, according to the method for manufacturing a glass thin film of the present invention, the intensities of the radiated light emitted from the substrate at a plurality of wavelengths are respectively detected when the porous thin film is formed. At the same time, the composition of the porous thin film to be formed on the substrate is controlled by adjusting the conditions for the production of glass particles and the deposition of glass particles according to this result. Therefore, the accuracy of measuring the composition of the porous thin film during formation can be improved, and a glass thin film having a desired composition can be provided.

Further, according to the apparatus for producing a glass thin film of the present invention, when the porous thin film is formed, the detecting means detects the intensities of the radiated light emitted from the substrate at a plurality of wavelengths, respectively, and the composition The control means controls the flame deposition means according to the detection result of the detection means to control the composition of the porous thin film to be formed on the substrate.
Therefore, the accuracy of measuring the composition of the porous thin film during formation can be improved, and a glass thin film having a desired composition can be provided.

[Brief description of drawings]

FIG. 1 is a diagram showing a conventional glass thin film manufacturing apparatus.

FIG. 2 is a perspective view of an apparatus for manufacturing a glass thin film according to an embodiment.

FIG. 3 is a side view of the glass thin film manufacturing apparatus of the embodiment.

FIG. 4 is a diagram showing a main part of a control system of a glass thin film manufacturing apparatus of an example.

FIG. 5 is a diagram showing an emission spectrum of a glass fine particle layer.

FIG. 6 is a diagram showing the relationship between the intensity of each emission peak and the concentration of each component.

[Explanation of symbols]

11 ... Substrate, 12, 13 ... Flame deposition means, 16 ... Reaction vessel, 18, 19 ... Detection means, 30 ... Composition control means.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Haruhiko Aikawa 1 Taya-cho, Sakae-ku, Yokohama-shi, Kanagawa Sumitomo Electric Industries, Ltd. Yokohama Works (72) Satoshi Hirose 1 Taya-cho, Sakae-ku, Yokohama, Kanagawa Sumitomo Denki Kogyo Co., Ltd. Yokohama Works (72) Inventor Masahide Saito 1 Taya-cho, Sakae-ku, Yokohama-shi, Kanagawa Sumitomo Denki Kogyo Co., Ltd. Yokohama Works

Claims (2)

[Claims] 1. A raw material is supplied together with an oxyhydrogen flame into a reaction vessel to generate glass fine particles, the glass fine particles are deposited on a substrate to form a porous thin film, and then the substrate is heated at a high temperature. In the method of manufacturing a glass thin film for making the porous thin film transparent, in forming the porous thin film, the intensities of the radiated light emitted from the substrate are detected at a plurality of wavelengths, respectively, and are detected. And controlling the composition of the porous thin film to be formed on the substrate by adjusting the conditions of the production of the glass fine particles and the deposition of the glass fine particles according to the intensity ratio of the emitted light at the plurality of wavelengths. A method for producing a glass thin film, comprising: 2. A flame deposition means for supplying a raw material together with an oxyhydrogen flame into a reaction vessel to generate glass fine particles, and depositing the glass fine particles on a substrate to form a porous thin film, said porous material. When forming a thin film in the shape of a detector, each detecting the intensity of the emitted light emitted from the substrate at a plurality of wavelengths, according to the intensity ratio of the emitted light detected by the detector at the plurality of wavelengths, An apparatus for producing a glass thin film, comprising: a composition control unit that adjusts a flame deposition unit to control the composition of a porous thin film to be formed on the substrate.