JPS6169961A - Nozzle for apparatus for manufacturing thin film by atomization - Google Patents

Abstract

PURPOSE:To eject a uniformly atomized soln. of starting material by placing a filter having many through holes between a hole for introducing an atomized soln. of starting material and a hole for ejecting the soln. CONSTITUTION:A filter 14 for mist diffusion having many through holes is placed between a hole 13 for introducing mist of a soln. of starting material into a nozzle head 12 from a duct 11 and the ejecting hole 10 of the nozzle head 12. A spongy substance having through holes whose directions are irregular, a bundle of many slender glass pipes, finely latticed thin plates or the like is used as the filter 14. By this nozzle structure, a uniform thin film can be manufactured on the surface of a substrate.

Description

Detailed Description of the Invention [Industrial Application Field] This invention sprays an atomized raw material solution onto a heated substrate to form a 5n02. In2O3, TiO2, S
This invention relates to a nozzle used to spray atomized raw material solution onto a substrate in an apparatus for producing thin films such as i02.

[Conventional technology]

The configuration of this type of atomized thin film production apparatus will be explained with reference to FIG. 5. The substrate 2.2- are installed, and these are heated by heater 3 from the back side to 400 to 50
Heated to 0°C. In the case shown, these substrates 2.2-.
- is sent from the cloth to the left side in Figure 2. Substrate 2.2-
An atomizer 4 and an air supply device 5 are provided below the atomizer 4.
A nozzle 6 connected to is placed towards the substrate 2.2-.

A chloride solution of Sn, In, etc. is used as the raw material solution,
This is atomized in the atomizer 4.

A fan 9 provided in the air supply device 5 removes air from the nozzle 6 to the substrate 2.
, 2-... are sprayed gently onto the surface. A part of the mist-like raw material solution is heated near the surface of the substrates 2, 2...- to be dehydrated and vaporized, and reacts with oxygen and water vapor in the air to form the substrate 2.2- A thin film made of oxides of Sn, In, etc. is formed on the surface of the substrate.

In a conventional atomized thin film production apparatus, a nozzle 6 as shown in FIG. 5 is used. This nozzle 6 has a funnel-shaped nozzle head 12 connected to the tip of a conduit 11 connected to the atomizer 4 side, and the tip of the head 12 is wider than the substrates 2, 2... The discharge port 10 is rectangular.

[Problem that the invention seeks to solve]

However, in the nozzle 6, if the opening area of the discharge port 10 is wider than the flow path area of the conduit 11, the flow velocity of the mist discharged from the discharge port 10 will be particularly high at the extended portion of the conduit 11, and from now on The flow becomes non-uniform, as it gradually slows down as it moves away. In this case, the thin film formed on the surface of the substrate 2.2- also has non-uniformity in film thickness corresponding to this flow rate, causing a problem that it is difficult to form a uniform thin film.

The present invention has been made to solve the above-mentioned problems with the conventional nozzle 6, and the mist is discharged from the discharge port 10 of the nozzle 6 so uniformly that the substrate 2.2-・A thin film with a uniform state is formed.

[Means to solve the problem]

Hereinafter, the configuration of the present invention will be explained based on the embodiments shown in FIGS. A mist diffusion filter 14 having a large number of holes is provided between the filter 10 and the filter 10 .

A porous body having a large number of holes is used as the filter 14, and in FIG. 1, a spongy body with one hole in an irregular direction is used. On the other hand, the second
The one shown in the figure is made of a porous material with each hole having a certain direction, such as a bundle of thin glass tubes, a fine lattice of thin plates, or a honeycomb. There is. Furthermore, in FIG. 3, a porous body with nine pores in an irregular direction and a porous body with nine pores in a directional manner are superimposed, and the latter is placed on the discharge port 10 side.

[For production]

The mist sent from the conduit 11 to the nozzle 6 has a flow rate reduced in the nozzle head 12, which has a wider cross-sectional area than the conduit 11, and temporarily stagnates in front of the filter 14, where it is filled. Thereafter, the mist flows out from the through hole 11 of the filter 14 to the discharge port 10, so that the mist is uniformly and gently discharged from the discharge port 10. This allows the board 2.2
A uniform amount of the raw material solution is supplied to the surface of the nozzle along the width direction of the Rad 12, and a thin film of uniform thickness is produced.

Note that the filter 14 as shown in FIG. 1, which has holes without directionality, generally has a high mist diffusion effect, but has a high mist flow resistance, and the directionality of the mist discharged from the discharge port 10 is constant. It has the characteristic that it does not. On the other hand, a filter 14 as shown in FIG. 2 in which one hole has directionality generally has a relatively low mist diffusion effect, but conversely has a low flow resistance.

It also has the characteristic that the directionality of the ejected mist is uniform. Furthermore, a filter 14 as shown in FIG. 3 in which these two layers are superimposed has an intermediate property that combines these characteristics, and in particular, a layer having holes with the latter directionality is ejected. In the case of the one shown in FIG. 3, which is placed on the outlet 10 side, the directionality of the ejected mist is well aligned, making it easy to produce a uniform thin film.

〔Example〕

Next, examples and comparative examples of the present invention will be described.

(Example 1) 25 g of tin tetrachloride (trihydrate), antimony trioxide Ig,
A raw material solution was prepared by sequentially dissolving 5 ml of hydrochloric acid in 150 cc of pure water, and the raw material solution was put into the atomizer 4.

The substrate 2.2- has a thickness of 1 mm, On+, and 100 mm in length and width.
A glass substrate of No. m was used and heated from the back side with a heater 3. At this time, the surface temperature of the substrate 2.2- was about 400°C.

The nozzle 6 has a width of 1201 m and a length of 20 long discharge ports 10, and the nozzle head 12 has a diameter of 2 to 3 mm.
A filter 1 made of cordierite porous porcelain (porosity 85%) with a thickness of 20 m and having a large number of holes penetrating the front and back sides of the filter.
4 was established.

Board 2.2- from right to left in Figure 5 at 15 m/min.
At the same time, the raw material liquid was atomized at a rate of 1 ml per minute by the atomizer 4, and this was gently sprayed from the nozzle 6 onto the substrates 2, 2, etc., to form a thin film of tin oxide on the surface thereof. .

One of the substrates 2.2- on which the thin film was fabricated was designated as sample 1, and the film thickness at each point indicated by A-E in Fig. 6 on this surface was measured, and the maximum and minimum values were calculated. The difference δmax is shown in the attached table.

(Example 2) A porous body made by bundling a large number of glass tubes with an inner diameter of 2φ, an outer diameter of 3φ, and a length of 30wn is attached as a filter 14 to the same nozzle 6 as in Example 1, and the substrate 2 is
A thin film was fabricated on the surface of ,2.-.

Similarly, using one substrate 2 as sample 2, the difference δmax between the maximum and minimum film thickness measured at each point A-E shown in FIG.
are shown in the separate table.

(Example 3) The same nozzle 6 as in Example 1 above, the same cordierite porous porcelain as that used in the same example as the filter 14, with a thickness of 7 having a large number of regular holes with a -side of 5n.
A stack of porous bodies having a honeycomb structure with a length of 0 m was attached so that the latter became the discharge port 1011J, and a thin film was produced on the surface of the substrate 2.2- in the same manner as in the same example.

Similarly, using one substrate 2 as sample 3, the difference δmax between the maximum and minimum film thicknesses measured at each point A-E shown in FIG.
are shown in the separate table.

Appended Table Unit (μm) (Comparative Example) A thin film was produced on the surface of the substrate 2° 2- in the same manner as in Example 1 without attaching the filter 14 to the same nozzle 6 as in Example 1 above.

Similarly, using one substrate 2 as a comparative example, the difference δmax between the maximum and minimum film thickness measured at each point A-H shown in FIG.
are shown in the separate table.

As is clear from the attached table, in samples 1 and 3.

The film thickness variation δmax is extremely small, such as 0.003 μm and 0.014 μm for sample 2, whereas in the comparative example using a conventional nozzle.

A relatively large variation δ such as 0.180μm
I could see wax. The film thickness of these samples is 0.34
It was ~0.38 μm.

Note that the above examples are all for the case of producing a 5n02 film, but other thin films 1, such as In203. TiO
2. Approximately similar results can be obtained when producing a thin film such as Si02.

〔Effect of the invention〕

As explained above, according to the present invention, the atomized raw material liquid can be uniformly discharged from the discharge port 10 of the nozzle 6, so that a thin film in a uniform state can be produced on the surface of the substrate 2.2-. You will be able to do this.

[Brief explanation of the drawing]

1 to 3 are partially cutaway perspective views of a nozzle showing each embodiment of the present invention, FIG. 4 is a partially cutaway perspective view showing a conventional example of a nozzle, and FIG. 5 is a mist FIG. 6, an explanatory diagram showing an outline of the reduced thin film production apparatus, is a surface view of a substrate showing the film thickness measurement position in an embodiment of the present invention. 2. One board 4-Atomizer 5-Air supply device
6-Nozzle 1〇-Discharge port 11-Conduit 12--Nozzle head 13-Inlet 14- Filter patent applicant Director-General of the Agency of Industrial Science and Technology, Ministry of International Trade and Industry 1 Taiyo Yuden Co., Ltd. Representative Patent attorney Kazuyoshi Hojo Figure 5 6th [! 1 x x 11th! 1st 3rd chapter 21! 21 IP, 41! l

Claims (1)

[Claims] 1. An atomizer that atomizes a raw material solution and an air supply device that sends the atomized raw material solution to a nozzle are provided, and a substrate is installed with its surface facing downward; A nozzle is installed below the substrate, and the atomized raw material solution is gently sprayed from the nozzle onto the surface of the substrate while heating the substrate to form a thin film on the surface. Production of an atomized thin film characterized in that a filter for mist diffusion having a large number of fine holes is provided between an inlet through which mist is introduced into a wide nozzle head and an outlet of the same nozzle head. Nozzle for equipment. 2. The nozzle for an atomized thin film production device according to claim 1, wherein the filter is made of a porous body having a large number of holes with irregular orientation. 3. The nozzle for an atomized thin film production apparatus according to claim 1, which is made of a porous body having a large number of holes arranged in the direction in which the filter discharges mist. 4. The filter consists of two layers: a porous body with a large number of pores with irregular orientation, and a porous body with a large number of pores lined up in the direction in which the mist is discharged; The nozzle for an atomized thin film production apparatus according to claim 1, wherein the body is provided on the discharge port side of the nozzle head.