JP2872925B2 - Nozzle for ultra-fine particle lamination - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a nozzle for laminating ultrafine particles used for spraying aerosol ultrafine particles and laminating a film on a substrate surface.

[0002]

2. Description of the Related Art An ultrafine powder having a submicron particle diameter obtained by a plasma evaporation method, an in-gas evaporation method, a plasma CVD method, a solution spray pyrolysis method or the like is formed into an aerosol and sprayed on an appropriate substrate surface. And used as a film to impart a given function to the substrate. When spraying the ultrafine particles, a small-diameter nozzle having a tip of about 0.01 to 5 mm or a nozzle such as a parallel pipe is used. The ultrafine particles are sprayed toward the surface of the base material at a predetermined pressure, and are laminated on the surface.

[0003]

In a nozzle which has been used conventionally, the diameter of the nozzle is small, so that the laminated film formed on the surface of the base material tends to be dot-shaped. Therefore, a laminated film cannot be formed on a substrate having a large area at a time. Although lines can be drawn on the surface of the base material by moving the base material and / or the nozzle with the laminated film, it is necessary to move the line for the width of the line for a large area. Books must be drawn in parallel. For this reason, a portion where the lines of the laminated film overlap was inevitable, and the obtained laminated film was uneven, and a laminated film having a uniform film thickness could not be obtained.

[0004] When laminating ultrafine particles on a rod-shaped substrate, relative rotation of the substrate or the nozzle is required. For the relative movement, a method of reciprocating the nozzle or the substrate in the axial direction while rotating the substrate, a method of moving the nozzle or the substrate in the axial direction while rotating the nozzle around the rod-shaped substrate, and the like are adopted. I was Therefore, a driving mechanism of a complicated mechanism is required, which is a bottleneck for improving operability and productivity. The present invention has been devised in order to solve such a problem. By devising a nozzle shape, a complicated drive mechanism is not required, and even a substrate having a large area can be uniformly formed. An object is to form a laminated film with a film thickness.

[0005]

In order to achieve the object, a nozzle for laminating ultrafine particles according to the present invention has a supply pipe and a slit-shaped opening provided on a side surface of a distal end portion of the supply pipe and extending in a width direction. And a flat plate-shaped collision plate that covers the end face of the distal end and protrudes laterally from the distal end edge of the opening, and changes the flow of fine particles flowing inside the supply pipe so as to change the flow axis of the supply pipe. The angle of the collision plate with respect to is in the range of 60 to 90 degrees. A tapered portion for narrowing the flow of the fine particles into a flat shape may be provided between the supply pipe and the opening. The nozzle according to the present invention has, for example, as shown in FIG. 1, the opening at the tip of the nozzle formed in a long slit shape in the width direction, and a collision plate so that the flow of the jetted aerosol is bent at the outlet side.

FIG. 1A shows a supply pipe 1 having a cylindrical base end.
And the supply pipe 1 is a tapered portion 2 which is narrowed flat. An opening 3 is formed on the side of the distal end of the tapered portion 2, and a collision plate 4 is provided on the distal end side edge of the opening 3. The aerosol-like fine particles are supplied with energy in the direction of the tube axis when flowing through the supply tube 1. However, the energy in the direction of the tube axis is canceled by the collision plate 4 at the distal end, and the fine particles along the direction perpendicular to the tube axis. From the opening 3. FIG. 1B shows a nozzle in which an opening 3 is formed on the side surface of the distal end without narrowing the square pipe-shaped supply pipe 1. The supply pipe 1 is not limited to the cylindrical shape (a) or the square pipe shape (b), but can have any cross-sectional shape. Also,
The tapered portion 2 that flattens the flux of the fine particles passing through the supply pipe 1 is effective in making the fine particle flux at the nozzle outlet uniform. However, in a nozzle in which fine particles flow with a uniform density distribution in the supply pipe 1, the tapered portion 2 does not need to be particularly provided.

The nozzle can be made of various materials as long as it is inert to a carrier gas and ultrafine particles.
Specific examples include iron, steel, stainless steel, copper, copper alloys, other metals or alloys, resins such as acrylic, polyvinyl chloride, polyethylene, polystyrene, and polypropylene, ceramics, glass, and the like. The material of the nozzle is selected in consideration of the endurance of the atmosphere. For example, if the aerosol has heat, or if the substrate needs to be heated when laminating ultrafine particles, the nozzle will also be heated, so metals and ceramics with excellent heat resistance are used. You. The inner surface of the nozzle is preferably subjected to a surface treatment such as polishing, plating, and resin coating in order to prevent adhesion and deposition of ultrafine particles. The inner surface of the nozzle is improved in slipperiness with respect to fine particles by surface treatment, adhesion and deposition are prevented, and ultrafine particles can be smoothly sent out.

The gas ejected from the opening 3 has a sonic velocity of 30
As long as the surface is maintained at a flow rate of m / sec, the ultrafine particles are laminated over a wide area of the substrate. In this regard, the shape of the opening 3 is not particularly limited, but a slit-shaped opening 3 is preferable for forming a uniform laminated film on a rod-shaped base material or a large area. The angle of the collision plate 4 with respect to the tube axis is 60
If the degree is higher than that, ultrafine particles can be laminated on the surface of the substrate. However, when the angle of the collision plate 4 exceeds 90 degrees, the resistance against the flow of the fine particles increases, and the fine particles accumulate on the collision plate 4 itself. As a result, the stacking efficiency decreases. Therefore, it is necessary to provide the collision plate 4 at an angle of 60 to 90 degrees with respect to the tube axis.
The collision plate 4 needs to have a size that completely covers the vertical surface to the tube axis and completely changes the flow direction of the fine particles flowing through the supply tube 1. In the collision plate 4 which does not have a size to completely cover the vertical plane with respect to the tube axis, the fine particles blown out from the opening 3 also generate a flow along a direction parallel to the tube axis. As a result, the ejected fine particles are diffused, and the lamination efficiency on the surface of the base material is reduced.

[0009]

【Example】

Example 1 A nozzle according to the present invention was incorporated in an RF plasma apparatus, and ultrafine alumina particles were sprayed on a titanium substrate to investigate nozzle performance. The nozzle used was made of stainless steel SUS304, having a thickness of 1 mm, an outer diameter of the supply pipe 1 above the nozzle of 15 mm, a nozzle length of 50 mm, and an opening 3.
Slit shape 3mm x 20mm, nozzle bottom 5mm x
It was designed to be 20 mm. In the RF plasma apparatus, as shown in FIG. 2, alumina was supplied from the feeder 5 to the plasma generator 6 at a flow rate of 1 g / min. 85 as plasma gas
% Of Ar + 15% mixture gas of H ₂ is flowed into the plasma generating section 6 with 100 l / min flow rate, and plasma in output 40 kW. When alumina was introduced into the plasma, the alumina became ultrafine particles having a particle size of 1 μm or less. After the ultrafine particles are introduced into the cooling chamber 8 via the supply pipe 7, the laminating chamber 9 in which the internal pressure is maintained at 200 to 300 Torr.
Was sent to A nozzle 10 is installed in the stacking chamber 9 from above to below.
The titanium substrate 11 of mx 15 mm x 50 mm is opposed. The distance between the opening and the substrate 11 is set to 25 mm,
Lamination continued for 15 minutes.

When the laminated film formed on the substrate 11 was observed, a thickness of about 1 mm was formed on the surface having a width of 5 mm and a length of 20 mm.
mm was formed. The laminated film was relatively firmly and densely adhered to the substrate 11 to such an extent that the laminated film was not peeled off by a slight impact. Therefore, the substrate 11 after the lamination did not require special care in handling as long as no impact was applied. 3mm × 20 slit shape
mm and 1 mm x 20 mm nozzle 10 was used,
Alumina was laminated on the titanium substrate 11 under the same conditions.
Also in this case, a laminated film having a uniform thickness and excellent adhesion was formed on the surface of the substrate 11.

Example 2 As a substrate, a columnar titanium having a diameter of 3 mm and a length of 30 mm was used. The substrate was placed along the longitudinal direction of the nozzle opening, and alumina ultrafine particles were laminated under the same conditions as in Example 1 while rotating the substrate with a motor. After laminating for 15 minutes, the thickness is about 0.5mm
Was formed on the substrate surface.

Embodiment 3 The opening 3 of the nozzle 10 is turned downward as shown in FIG.
A titanium substrate 11 of mm × 50 mm was arranged. Motor 1
2, the alumina fine particles were reciprocated at a speed of 0.5 mm / sec and a stroke of 15 mm along the direction perpendicular to the longitudinal direction of the opening 3, and the alumina ultrafine particles were stirred for 40 minutes under the same conditions as in Example 1. Laminated. The surface of the substrate 11 after the laminating process has a thickness of 1 m in a range of 20 mm × 20 mm.
m was formed. This film is
The adhesion to No. 1 was good.

Embodiment 4: Impact plate 4 against nozzle tube axis
Was changed in the range of 45 to 120 degrees as shown in FIG. 4, and alumina ultrafine particles were laminated on a titanium substrate under the same conditions as in Example 1. With the nozzle having the collision plate attached at θ = 60 ° and θ = 90 °, a laminated film having a thickness of about 1 mm having excellent uniformity and adhesion was formed as in Example 1. However, in the case of using the nozzle with the collision plate 4 attached at θ = 45 degrees, almost no ultrafine particles were laminated on the substrate 11. When θ = 120 degrees, the collision plate 4
In the case of using the nozzle equipped with, the thickness of the laminated film was only about 0.5 mm.

Comparative Example: As shown in FIG. 5, as a nozzle, a cylindrical nozzle (a) having an outlet of 5 mm in diameter and a nozzle (b) having a 2 mm × 20 mm slit at the tip opening were used. Then, ultrafine alumina particles were laminated on the surface of the titanium substrate under the same conditions as in Example 1. In this case, the obtained laminated film had a thickness of about 0.01 to 0.05 mm, and efficient lamination of ultrafine particles as in the example could not be performed. In the nozzle (b) having a flat opening,
Although the shape of the opening was the same as that of the nozzle of the present invention, the aerosol flowed straight out of the nozzle, so that a thick film as in Example 1 could not be laminated. From the comparison between the comparative example and the example, it can be seen that changing the flow of the ultrafine particles ejected from the nozzle is effective for efficiently stacking the ultrafine particles on the substrate.

[0015]

As described above, the nozzle for laminating ultra-fine particles according to the present invention has a slit-shaped opening formed in the side surface of the nozzle tip, which is long in the width direction. It protrudes laterally from the tip side edge. Therefore, the aerosol of the ultrafine particles flowing in the nozzle is changed in flow direction by the collision plate, and flies to the surface of the base material. When the ultrafine particles are laminated in this manner, a laminated film having a uniform thickness over a wide area is efficiently formed. Also, by laminating the rod-shaped substrate while moving the nozzle and / or the substrate relatively, it is possible to laminate the rod-shaped substrate to a uniform thickness.

[Brief description of the drawings]

FIG. 1 shows two examples of a nozzle for laminating ultrafine particles according to the present invention.

FIG. 2 shows an example in which a nozzle according to the present invention is incorporated in an RF plasma device.

FIG. 3 shows a state in which ultrafine particles are laminated while reciprocating the substrate.

FIG. 4 is a view for explaining Example 4 in which the effect of the inclination angle of the collision plate with respect to the tube axis on the deposition of ultrafine particles was investigated.

FIG. 5 shows two examples of a conventional nozzle having an opening formed at the end face of the tip.

[Explanation of symbols]

1: supply pipe 2: tapered section 3: opening 4: collision plate 5: feeder 6: plasma generation section 7: supply pipe 8: cooling chamber
9: Laminating chamber 10: Nozzle 11: Substrate 1
2: Motor θ: Angle of impact plate with respect to tube axis

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-60-75347 (JP, A) JP-A-4-267958 (JP, A) Fully open 1983-55506 (JP, U) Really open 1983 43959 (JP, U) Fully open sho 59-158451 (JP, U) Fully open sho 60-74751 (JP, U) Full open 3-15654 (JP, U) Full open 5-56256 (JP, U) Japanese Utility Model Application Hei 5-56255 (JP, U) Japanese Utility Model Application Sho 61-864 (JP, U) Japanese Utility Model Application Sho 47-3352 (JP, Y1) (58) Fields investigated (Int. Cl. ⁶ , DB name) B05B 1/00-1/36

Claims (2)

(57) [Claims] 1. A supply pipe, a slit-shaped opening provided on a side surface of a distal end portion of the supply pipe and extending in a width direction, and covering an end surface of the distal end portion, and protruding laterally from a distal end side edge of the opening portion. An ultra-fine particle laminating nozzle having a flat plate-like collision plate, wherein the angle of the collision plate with respect to the tube axis of the supply tube is in the range of 60 to 90 degrees so as to change the flow of the fine particles flowing inside the supply tube. 2. The ultrafine particle laminating nozzle according to claim 1, wherein a tapered portion for narrowing the flow of the fine particles into a flat shape is provided between the supply pipe and the opening.