JPH08173851A - Nozzle for laminating ultrafine particles - Google Patents

Abstract

PURPOSE: To laminate ultrafine particles with high lamination efficiency even on the surface of a base material having wide area or a bar-like base material. CONSTITUTION: A slit-shaped opening 3 extending in the breadth direction is provided on the side of the tip of a feeding pipe 1, and an impact plate 4 covering the end surface of the tip is protruded sideways from the edge part on the tip end side of the opening 3. An angle of the impact plate to the pipe axis of the feeding pipe 1 is set in the range of 60-90 deg.C. Between the feeding pipe 1 and the opening 3, a tapered part 2 for throttling the flow of ultrafine particles flatly may be installed. Therefore, the flow of the ultrafine particles flowing inside the feeding pipe 1 is changed by the impact plate 4 to laminate the ultrafine particles over the wide area of a base material.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ultrafine particle laminating nozzle which is used when aerosol ultrafine particles are sprayed to form a film on the surface of a substrate.

[0002]

2. Description of the Related Art Ultrafine powder having a submicron particle size obtained by a plasma evaporation method, a gas evaporation method, a plasma CVD method, a solution spray pyrolysis method or the like is made into an aerosol and sprayed on an appropriate substrate surface. And is used as a coating that imparts a given function to the substrate. At the time of spraying the ultrafine particles, a small diameter nozzle having a diameter of about 0.01 to 5 mm or a nozzle such as a parallel pipe is used. The ultrafine particles are jetted toward the surface of the base material at a predetermined pressure and are laminated on the surface.

[0003]

In the conventionally used nozzle, since the nozzle diameter is small, the laminated film formed on the surface of the base material is likely to be dot-shaped. Therefore, a laminated film cannot be formed at once on a substrate having a large area. Although it is possible to draw a line with the laminated film on the surface of the substrate by moving the base material and / or the nozzle, it is necessary to move the line width for each large area. I have no choice but to draw books in parallel. Therefore, the portion where the lines of the laminated film overlap is inevitable, and the obtained laminated film has unevenness, so that the laminated film having a uniform film thickness cannot be obtained.

Further, when laminating ultrafine particles on a rod-shaped base material, relative rotation of the base material or the nozzle is required. For the relative movement, a method of reciprocating the nozzle or the base material in the axial direction while rotating the base material, a method of moving the nozzle or the base material in the axial direction while rotating the nozzle around the rod-shaped base material, etc. are adopted. Was there. Therefore, a driving mechanism having a complicated mechanism is required, which is a bottleneck in improving operability and productivity. The present invention has been devised to solve such a problem, and by devising the nozzle shape, a complicated drive mechanism is not required and even a base material having a large area can be made uniform. The purpose is to form a laminated film with a film thickness.

[0005]

In order to achieve the object, an ultrafine particle laminating nozzle of the present invention is provided with a supply pipe and a slit-shaped opening provided in a side surface of a front end portion of the supply pipe and widened in a width direction. And a flat plate-like collision plate that covers the end face of the tip portion and projects laterally from the edge portion on the tip end side of the opening, and changes the flow of fine particles flowing inside the feed pipe so that the tube axis of the feed pipe is changed. The angle of the collision plate with respect to is in the range of 60 to 90 degrees. A taper portion that narrows the flow of 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, a nozzle end opening formed in a slit shape that is long in the width direction, and is provided with a collision plate so that the flow of ejected aerosol is bent on the outlet side.

FIG. 1A shows a supply pipe 1 having a cylindrical base end side.
And the supply pipe 1 is a flattened tapered portion 2. An opening 3 is formed on the tip side surface of the tapered portion 2, and a collision plate 4 is provided on the tip side edge of the opening 3. The aerosol-shaped fine particles are given energy in the tube axis direction when flowing through the supply tube 1, but the energy in the tube axis direction is canceled by the collision plate 4 at the tip portion, and the particles along the direction orthogonal to the tube axis. And is ejected from the opening 3. FIG. 1B shows a nozzle in which an opening 3 is formed on a side surface of a tip without squeezing 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 may have any cross-sectional shape. Also,
The taper portion 2 that flattens the flux of fine particles passing through the supply pipe 1 is effective in making the flux of fine particles at the nozzle outlet uniform. However, in a nozzle in which fine particles flow in the supply pipe 1 with a uniform density distribution, it is not necessary to provide the tapered portion 2 in particular.

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

The gas ejected from the opening 3 has a sound velocity of -30.
As long as the surface is maintained at a flow rate of m / sec, ultrafine particles are laminated on a large area of the substrate. In this respect, the shape of the opening 3 is not particularly limited, but the slit-shaped opening 3 is preferable in order to form a uniform laminated film for a rod-shaped base material or a large area. The angle of the collision plate 4 with respect to the tube axis is 60
When it is more than 100 degrees, the ultrafine particles can be laminated on the surface of the base material. However, when the angle of the collision plate 4 exceeds 90 degrees, the resistance against the flow of fine particles increases, and the fine particles accumulate on the collision plate 4 itself. As a result, the stacking efficiency decreases. Therefore, the collision plate 4 needs to be provided 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 with respect to the tube axis and completely changes the flow direction of the particles flowing through the supply tube 1. In the collision plate 4 that does not have a size that completely covers the vertical surface with respect to the tube axis, the fine particles blown out from the opening 3 also have a flow in a direction parallel to the tube axis. As a result, the ejected fine particles are diffused and the stacking efficiency on the surface of the base material is reduced.

[0009]

【Example】

Example 1: A nozzle according to the present invention was incorporated into an RF plasma device, and ultrafine particles of alumina were sprayed onto a titanium substrate to investigate the nozzle performance. The nozzle used is made of stainless steel SUS304 and has a wall 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
Designed to be 20 mm. In the RF plasma device, as shown in FIG. 2, alumina was introduced from the feeder 5 into the plasma generation part 6 at a flow rate of 1 g / min. 85 as plasma gas
A mixed gas of% Ar + 15% H ₂ was caused to flow into the plasma generation part 6 at a flow rate of 100 liter / min, and plasma was generated at an output of 40 kW. When alumina was introduced into this plasma, the alumina became ultrafine particles having a particle size of 1 μm or less. The ultrafine particles are introduced into the cooling chamber 8 through the supply pipe 7, and then the laminating chamber 9 whose internal pressure is maintained at 200 to 300 Torr.
Was sent to. A nozzle 10 is installed in the stacking chamber 9 from the upper side to the lower side, and the nozzle 10 has an opening of 5 m.
The titanium substrates 11 of m × 15 mm × 50 mm are opposed to each other. Set the distance between the opening and the substrate 11 to 25 mm,
Lamination was continued for 15 minutes.

Observation of the laminated film formed on the substrate 11 revealed that the thickness was about 1 mm on the surface having a width of 5 mm and a length of 20 mm.
A uniform laminated film of mm was formed. The laminated film was relatively firmly and densely adhered to the substrate 11 so as not to be peeled off by some impact. Therefore, the laminated substrate 11 did not require any special handling as long as no impact is applied. 3mm x 20 slit shape
mm and 1 mm × 20 mm nozzle 10 is used,
Alumina was laminated on the titanium substrate 11 under the same conditions.
In this case as well, a laminated film having a uniform thickness and excellent adhesion was formed on the surface of the substrate 11.

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

Example 3: The opening 3 of the nozzle 10 is directed downward as shown in FIG. 3, and 5 mm × 50 is placed below the opening 3.
A titanium substrate 11 of mm × 50 mm was arranged. Motor 1
2, while reciprocating the substrate 11 at a speed of 0.5 mm / sec and a stroke of 15 mm along the direction orthogonal to the longitudinal direction of the opening 3, the alumina ultrafine particles were for 40 minutes under the same conditions as in Example 1. Laminated. The surface of the substrate 11 after the lamination process has a thickness of 1 m within a range of 20 mm × 20 mm.
A uniform film of m was formed. This film is also the substrate 1
The adhesion to 1 was good.

Example 4: Collision plate 4 against nozzle tube axis
The angle θ was changed in the range of 45 to 120 degrees as shown in FIG. 4, and the ultrafine alumina particles were laminated on the titanium substrate under the same conditions as in Example 1. With the nozzle equipped with the collision plate at θ = 60 degrees and θ = 90 degrees, a laminated film having a thickness of about 1 mm, which was excellent in uniformity and adhesiveness, was formed as in Example 1. However, in the case of using the nozzle to which the collision plate 4 is attached at θ = 45 degrees, the ultrafine particles were hardly laminated on the substrate 11. Also, the collision plate 4 at θ = 120 degrees
The thickness of the laminated film was only about 0.5 mm when the nozzle equipped with was used.

Comparative Example: As the nozzle, as shown in FIG. 5, a cylindrical nozzle (a) having a diameter of 5 mm and a nozzle (b) having a tip opening narrowed into a slit of 2 mm × 20 mm were used. Then, under the same conditions as in Example 1, ultrafine alumina particles were laminated on the surface of the titanium substrate. In this case, the obtained laminated film had a thickness of about 0.01 to 0.05 mm, and it was not possible to efficiently laminate the ultrafine particles as in the example. In the nozzle (b) with 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 from the nozzle, so that the thick film as in Example 1 could not be laminated. From the comparison between the comparative example and the example, it is understood 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, in the nozzle for laminating ultrafine particles of the present invention, a slit-shaped opening that is long in the width direction is formed on the side surface of the nozzle tip, and the collision plate that closes the nozzle tip is formed in the opening. It projects laterally from the front edge. Therefore, the aerosol of the ultrafine particles that has flowed through the nozzle has its flow direction changed 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 large area is efficiently formed. In addition, even with respect to the rod-shaped base material, by stacking the nozzle base material and / or the base material while moving the base material relatively, it is possible to stack the base material with a uniform thickness.

[Brief description of 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 A state in which ultrafine particles are laminated while the substrates are reciprocally moved.

FIG. 4 is a diagram illustrating Example 4 in which the influence of the inclination angle of the collision plate with respect to the tube axis on the lamination of ultrafine particles was investigated.

FIG. 5 is an example of two conventional nozzles having an opening formed on the end face of the tip.

[Explanation of symbols]

1: Supply pipe 2: Tapered part 3: Opening part 4: Collision plate 5: Feeder 6: Plasma generation part 7: Supply pipe 8: Cooling chamber
9: Laminating chamber 10: Nozzle 11: Substrate 1
2: Motor θ: Angle of collision plate with respect to tube axis

Claims (2)

[Claims] 1. A supply pipe, a slit-shaped opening provided in a side surface of a front end portion of the supply pipe and widened in a width direction, and covers an end face of the front end, and projects laterally from a front end side edge portion of the opening. And a flat plate-like collision plate, wherein the angle of the collision plate with respect to the tube axis of the supply pipe is in the range of 60 to 90 degrees so as to change the flow of the fine particles flowing inside the supply pipe. 2. The ultrafine particle laminating nozzle according to claim 1, wherein a taper portion for narrowing the flow of the fine particles into a flat shape is provided between the supply pipe and the opening.