JPH0444595Y2 - - Google Patents

Description

[Detailed Description of the Invention] (Industrial Application Field) The present invention relates to a silicon oxide film manufacturing device for forming a silicon oxide film on the surface of a substrate. A treatment liquid circulating flow type suitable for maintaining the temperature of a treatment liquid containing an acid aqueous solution (hereinafter referred to as treatment liquid) at an appropriate temperature and forming a uniform silicon oxide film on the surface of a substrate immersed in the treatment liquid. The present invention relates to an apparatus for manufacturing a silicon oxide film.

(Prior art) The present applicant has filed an earlier application (Japanese Patent Application Laid-Open No. 60-33233
In Japanese Utility Model Application Publication No. 168574/1983), a method and apparatus for manufacturing a silicon oxide film were disclosed.

These include a processing tank installed in a thermostatic chamber, and the processing tank is divided into an immersion section for immersing the substrate, a rectification section for adjusting the flow of the processing liquid flowing into the immersion section, and a processing liquid adjustment section for regulating the processing solution flowing out from the immersion section. The present invention relates to a manufacturing method and a manufacturing apparatus for forming a uniform silicon oxide film on the surface of a substrate immersed in the immersion section while circulating the treatment liquid through each section. It has become possible to efficiently produce a silicon oxide film with a low haze rate.

In addition, in the above-mentioned silicon oxide film manufacturing apparatus, the temperature of the processing liquid circulating through each part in the processing tank is as follows:
The temperature is maintained at an appropriate temperature (35℃) by hot water stored in a constant temperature bath.

(Problems to be solved by the invention) However, in the above-mentioned manufacturing equipment, since the treatment tank uses a resin material such as vinyl chloride in consideration of contact with hydrosilicic acid, It is not recommended to heat the hot water in the thermostatic chamber above 50℃ (ideally, 40℃ or below is preferable).
As the volume of the processing tank expands as manufacturing equipment becomes larger, the amount of heat dissipated from the processing liquid from the opening of the processing tank increases.Especially in the winter when the surrounding temperature drops, the amount of heat released by the heated water in the constant temperature tank increases. There was a problem in that it was difficult to maintain the temperature of the treatment liquid at an appropriate temperature by heating alone, and the rate of formation of the silicon oxide film deposited on the surface of the substrate immersed in the treatment liquid became unstable.

The present invention was developed in view of the above-mentioned problems, and its purpose is to maintain the hot water in the thermostatic chamber at 40°C or lower even when the surrounding temperature is 10°C or lower. It is an object of the present invention to provide a silicon oxide film manufacturing apparatus that can maintain the temperature of a liquid at an appropriate temperature.

(Means for Solving the Problems) In order to achieve the above object, the present invention includes a treatment tank for storing a saturated silicon oxide aqueous solution of hydrosilicofluoric acid (hereinafter referred to as treatment liquid) in a constant temperature bath, The treatment tank includes an immersion section for immersing the substrate to form a silicon oxide film on the surface of the substrate, and a rectifier connected to the immersion section for adjusting the flow of the treatment liquid flowing into the immersion section. A silicon oxide film manufacturing apparatus comprising a processing liquid adjustment section connected to the immersion section for adjusting the processing liquid flowing out from the immersion section, and a circulation device for circulating the processing liquid. The method is characterized in that heating means and/or heat retention means for keeping the temperature of the processing liquid at an appropriate temperature are provided above the processing tank.

(Function) According to the silicon oxide film manufacturing apparatus according to the present invention, the heating means and/or
Alternatively, since a heat-retaining means is installed above the processing tank, even when the surrounding temperature drops below 10°C, the temperature of the processing liquid can be maintained at an appropriate temperature by keeping the temperature of the hot water in the constant temperature tank below 40°C. In addition, vinyl chloride can be used as the material for the treatment tank.

(Example) An example of the present invention will be described below with reference to the accompanying drawings.

FIG. 1 is a schematic diagram showing the configuration of a silicon oxide film manufacturing apparatus according to an embodiment of the present invention. FIG. 2 is a schematic side view of FIG. 1.

According to FIGS. 1 and 2, the silicon oxide coating manufacturing apparatus consists of a double tank, a constant temperature bath 1 and a treatment bath 2. Hot water 4 for heating the stored processing liquid 3 is stored. The constant temperature bath 1 is provided with a heater 5 for adjusting the temperature of the hot water 4 and a stirrer 6 used for stirring the hot water 4.

The processing tank 2 includes a dipping section 8 in which the substrate 7 is immersed, a treatment liquid adjustment section 10 provided next to the dipping section 8 with the dipping section 8 and a wall 9 separated, and a dipping section 10 separating the dipping section 8 and the wall 11 and immersing the substrate 7 therein. It consists of a rectifying section 13 provided with a tabular rectifying plate 12 having a large number of slits provided as a bottom plate of the section 8 as a boundary.

The processing liquid adjusting section 10 is provided with a stirrer 14 for homogenizing the processing liquid 3 and a processing liquid adjusting device 15a used for adding an aqueous boric acid solution to the processing liquid 3. A water pipe 15 is provided from the bottom of the treatment liquid adjustment section 10 to guide the treatment liquid 3 adjusted in the treatment liquid adjustment section 10 to the rectification section 13 .

The water pipe 15 once passes through the thermostatic chamber 1, is led to the outside, and is connected to the upper part of the rectifier 13. A processing liquid filtration filter 16 and a water pump 17 are provided in the middle of the water pipe 15 at positions that protrude to the outside of the thermostatic chamber 1 .

According to the above-described configuration, the processing liquid 3 stored in the processing liquid adjustment section 10 passes through the water pipe 15, the processing liquid filtration filter 16, is guided to the upper part of the rectification section 13, and is further section 8 and the processing liquid adjusting section 10.

As a means for keeping the processing liquid 3 at an appropriate temperature, a lid 18 is provided at the openings of the constant temperature bath 1 and the processing tank 2 to prevent heat radiation from the processing liquid 3 and hot water 4. An infrared lamp 19 is provided above the lid 18 to heat the lid 18 by radiation.

Note that 20 is a heat exchanger provided in the rectifier 10, and the heat exchanger 20 has a conduit 21 for guiding the heat medium.
A pump 22 is provided in the middle of the conduit 21 to send the heat medium to the heat exchanger 20. Generally, hot water, steam,
Although silicone oil or the like is used, in this embodiment, hot water 24 stored in a constant temperature bath 23 is used, and the hot water 24 is sent to a heat exchanger 20 by the power of a pump 22, and heat exchange is performed in the heat exchanger 20. The processing liquid 3 is heated.

Next, the operation of the silicon oxide film manufacturing apparatus of this embodiment will be explained.

First, as treatment liquid 3, a hydrosilicofluoric acid solution in which silicon oxide (silica gel) was saturated with 2 mol/hydrosilicic acid was prepared. This treatment liquid 3 is put into the treatment tank 2, and the water supply pump 21 is operated to increase the water supply amount (circulation amount) per minute to 8% of the total amount of treatment liquid.
It was set to

The processing liquid 3 is guided from the lower part of the processing liquid adjustment section 10 of the processing tank 2 into the water pipe 15 by the force of the water pump 17, passes through the processing liquid filtration filter 16, and then passes through the water pipe 15 for treatment. Rectifier 1 in tank 2
Sent to the top of 3. The processing liquid 3 sent to the rectifying section 13 passes through the hole in the rectifying plate 12 located at the boundary between the rectifying section 13 and the immersing section 8 and flows into the immersing section 8 . The processing liquid 3 becomes a substantially laminar flow in the immersion part 8 and flows vertically from below to above, and then crosses the wall 9 between the immersion part 8 and the processing liquid adjustment part 10 and flows into the processing liquid adjustment part 1.
Flows into 0. In the processing liquid adjustment section 10, 0.5
A boric acid aqueous solution having a concentration of 1 mol/molar is continuously added dropwise at a rate of 0.2 ml/min using the treatment liquid adjusting device 15, and is stirred using the stirrer 14 to form the treatment liquid 3.
equalize the concentration of

In addition, the heater 5 and stirrer 6 in the thermostatic chamber 1 are operated, and the infrared lamp 19 provided above the lid 18 is activated to heat the lid 18 to 35°C to 40°C by radiation. moreover,
The pump 22 is operated and the heat exchanger 20 provided in the rectifier 13 is operated to raise the temperature of the processing liquid 3 to 35
℃ and homogenized.

Maintain the above-mentioned state of addition of the boric acid aqueous solution for 15 hours,
The treatment liquid 3 was a supersaturated silicon oxide solution. In this treatment liquid 3, the base material 7, which had been thoroughly washed and dried after being immersed in a 0.5 wt% HF aqueous solution for 10 minutes, was immersed.
The temperature was maintained for 4 hours while continuing to circulate the treatment solution 3 and add the boric acid aqueous solution.

After 4 hours had elapsed, when the substrate 7 that had been immersed was pulled up, a silicon oxide film had been formed on the surface of the substrate 7.

As described above, in this embodiment, the processing liquid circulating flow type silicon oxide coating manufacturing apparatus is provided with a lid 18 that closes the openings of the constant temperature bath 1 and the processing bath 2. infrared lamp 19
The temperature of the lid body 18 is set at 35℃ to 40℃ by radiation.
Since the heating is performed at a temperature of 100.degree., heat radiation of the processing liquid 3 and hot water 4 from the upper portions of the constant temperature bath 1 and the processing bath 2 can be prevented.

Therefore, even if the ambient temperature drops below 10°C, the temperature of the processing liquid 3 can be maintained at 35°C, and the temperature of the processing liquid 3 stored in the immersion section 8 is also uniform between the upper and lower parts. Therefore, the film formation rate of the silicon oxide film deposited on the surface of the base material 7 became stable.

In addition, even if the temperature of the hot water in thermostatic bath 1 is kept below 40℃, the temperature of processing liquid 3 can be maintained at 35℃, so vinyl chloride is sufficient as the material for treatment bath 2. can do.

In the present embodiment, the lid 18 and the infrared lamp 19 are used as heating means and/or heat retention means to keep the temperature of the processing liquid 3 at an appropriate temperature, but other heating means and/or heat retention means are used. Alternatively, the heat-retaining means may include keeping the water pipe 15 warm to prevent heat radiation from the processing liquid 3, or heating the water pipe 15 to heat the processing liquid 3.

(Effects of the invention) As is clear from the above explanation, according to the silicon oxide film manufacturing apparatus according to the present invention, the heating means and/or heat retention means for keeping the processing liquid in the processing tank at an appropriate temperature are installed in the processing tank. Because it is installed above, even when the surrounding temperature drops to 10℃ or less, the temperature of the hot water in the constant temperature bath can be kept below 40℃, and the temperature of the processing liquid in the treatment tank can be maintained at an appropriate temperature. The temperature of the treatment solution becomes uniform between the upper layer and the lower layer, the rate of formation of the silicon oxide film deposited on the surface of the substrate becomes stable, and vinyl chloride can be used as the material for the treatment tank.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram showing the configuration of a silicon oxide film manufacturing apparatus according to an embodiment of the present invention, and FIG. 2 is a schematic side view of FIG. 1. In the drawing, 1 is a constant temperature bath, 2 is a treatment tank, 3 is a treatment liquid, 7 is a base material, 8 is an immersion part, 10 is a treatment liquid adjustment part, 13 is a rectification part, 15 is a water pipe, and 16 is a treatment liquid. A filtration filter, 17 a water pump, 18 a lid, and 19 an infrared lamp.

Claims (1)

[Scope of Claim for Utility Model Registration] (1) A treatment tank is provided in which a saturated silicon oxide aqueous solution of hydrosilicofluoric acid (hereinafter referred to as treatment liquid) is stored in a constant temperature bath, and the treatment tank is used to immerse a substrate. an immersion section for forming a silicon oxide film on the surface of the substrate; a rectification section connected to the immersion section to regulate the flow of the processing liquid flowing into the immersion section; In a silicon oxide coating manufacturing apparatus comprising a treatment liquid adjusting section connected to the immersion section for adjusting the treatment liquid and a circulation device for circulating the treatment liquid, the temperature of the treatment liquid is controlled. An apparatus for producing a silicon oxide film, characterized in that it is equipped with a heating means and/or a heat retaining means above the processing tank for maintaining the temperature at an appropriate temperature. (2) The apparatus for producing a silicon oxide film according to claim 1, wherein the heating means is an infrared lamp. (3) The apparatus for producing a silicon oxide film according to claim 1, wherein the heat retaining means is a lid that closes the opening of the thermostatic chamber and the processing chamber.