JPH0665757A - Formation of particulate film by gas deposition and forming device therefor - Google Patents

Abstract

PURPOSE:To provide the method for formation of a particulate film by a gas deposition method for forming the particulate having good adhesion to a substrate and the improved density free from flocs and the forming device therefor. CONSTITUTION:This method for formation of the particulate film consists in transporting the particulates formed by an evaporating source 7 to a rectilinear state by using a rectilinear transporting pipe 3 at the time of transporting the above-mentioned particulates together with a carrier gas onto a substrate 13. This particulate film forming device by the gas deposition method consists in forming the transporting pipe 3 connecting a particulate forming chamber 1 and a film forming chamber 2 to a rectilinear state without having a bend in the middle between the part above the evaporating source 7 and the substrate 13.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a fine particle film by a gas deposition method and an apparatus for forming the same.

[0002]

2. Description of the Related Art Conventionally, as a forming apparatus of this type, for example, as shown in FIG. 6, a fine particle generating chamber c provided with an evaporation source b for heating and evaporating a fine particle film material a, and a fine particle generating chamber c Conveying pipe d for conveying fine particles together with carrier gas
And a nozzle e connected to the tip of the carrier pipe d, and a fine particle film f formed by injecting fine particles and carrier gas from the nozzle e.
And a film forming chamber h in which a movable substrate g for forming a film is arranged. The particle forming chamber c and the film forming chamber h are arranged on the same plane. The transfer pipe d disposed between the transfer pipe d and the curved portion j which is largely bent near the carry-in port i of the transfer pipe d for transferring the fine particles generated from the evaporation source b to the film forming chamber h side together with the carrier gas. There is known a forming apparatus having, for example, a substantially U-shaped carrier pipe d having a bent portion k that is largely bent near the base portion of a nozzle e that injects the fine particles conveyed with the gas together with a gas. In the figure, m is a needle valve connected to a gas supply source n for supplying a carrier gas into the fine particle production chamber c, o is a heating device for the evaporation source b, and p is connected to the film forming chamber h via a valve q. A vacuum pump is shown.

When forming a fine particle film by the apparatus shown in FIG. 6, first, the evaporation source b in the fine particle generating chamber c is formed.
For example, Au is filled as the fine particle film material a. Subsequently, a predetermined amount of helium gas as a carrier gas is introduced from the gas supply source n into the particle generation chamber b by the needle valve m, and the evaporation source b is heated by supplying electric power of 430 W by the heating device o, Au of the film material in the evaporation source b
Is heated and melted and evaporated to produce Au fine particles. Next, the inside of the film forming chamber h is evacuated by the vacuum pump p, and A in the particle forming chamber c is generated by the pressure difference between the particle forming chamber c and the film forming chamber h.
u The fine particles are carried together with the carrier gas by the carrying pipe d into the film forming chamber h, and are moving at a constant speed from the nozzle e (arrow x direction).
The Au fine particles are jetted together with the carrier gas onto the substrate g to form the Au fine particle film f on the substrate g.

[0004]

In the conventional apparatus for forming a fine particle film by the gas deposition method, the fine particle generating chamber c is used.
Since the film forming chamber h and the film forming chamber h are arranged on the same plane, the transfer pipe d connecting the evaporation source in the particle generation chamber c and the substrate g in the film forming chamber h is located near the carry-in port i of the transfer pipe d. Curved part j,
Since there is a bent portion k near the base of the nozzle e, the bending of the bent portions j and k of the carrier pipe d causes turbulence in the gas flow of the carrier gas, resulting in collision of fine particles with each other during the carrier process. Larger aggregates are formed when the number of the transported fine particles of (3) increases. Since this aggregate causes deterioration of film quality such as adhesion to the substrate g, there is a problem that the fine particle deposition film is separated from the substrate.

The present invention is based on the gas deposition method which solves the above-mentioned problems, and when the fine particles are conveyed, the flow of gas can be prevented from being disturbed and the fine particles can be conveyed without causing agglomeration due to collision between the fine particles. An object of the present invention is to provide a method for forming a fine particle film and a forming apparatus used for forming the film.

[0006]

The present invention proposes a method for forming a fine particle film by a gas deposition method that achieves the above-mentioned object. A fine particle film is carried by a carrying tube together with a carrier gas, and this is carried by the carrying tube. In the gas deposition method of forming a fine particle film on a substrate by jetting from a nozzle at the tip of, the fine particles and carrier gas are conveyed by a linear conveying pipe between the evaporation source and the substrate.

Further, the present invention proposes an apparatus for forming a fine particle film by a gas deposition method for carrying out the above-mentioned forming method, wherein the fine particle film material evaporation source, the substrate, and the fine particles together with the carrier gas. In the apparatus for forming a fine particle film by the gas deposition method, which comprises a transport pipe for transporting fine particles of a film material, and a nozzle provided at the tip of the transport pipe for injecting a fine particle and a carrier gas onto a substrate, the transport pipe is It is characterized in that it is a carrier pipe formed in a straight line without bending between the evaporation source and the substrate. Further, an adjusting mechanism for adjusting the relative position between the evaporation source and the carry-in port of the carrier pipe may be provided, or a discharge port for discharging the surplus particles may be provided near the carry-in port of the carrier pipe.

[0008]

The fine particles are carried together with the carrier gas and jetted from the nozzle onto the substrate to be deposited to form a fine particle film. At that time, since the fine particles are conveyed in a straight traveling state together with the carrier gas through the linear conveying pipe, the gas flow is not disturbed during the conveyance, and therefore the fine particles do not aggregate.

[0009]

Embodiments of the present invention will be described with reference to the accompanying drawings. FIG. 1 shows an example of a forming apparatus for carrying out the present invention. In the figure, 1 is a fine particle generating chamber, 2 is a film forming chamber, and 3 is a space between the fine particle generating chamber 1 and the film forming chamber 2. The carrier pipe is shown.

A carrier gas made of, for example, helium gas can be introduced from a gas supply source 5 through a needle valve 6 from a gas introduction pipe 4 communicating with the fine particle production chamber 1. Further, an evaporation source 7 consisting of an alumina-coated tungsten basket having an opening diameter of 15 mm for accommodating the fine particle film material M to be heated and evaporated is provided in the fine particle generation chamber 1, and the evaporation source 7 is used as an evaporation source heating device. Connected to 8. Further, one end of a transfer pipe 3 having an inner diameter of 0.5 mm for transferring the fine particles together with a carrier gas is airtightly inserted and connected to the inside of the fine particle generation chamber 1, and a stainless steel inner diameter of 0.5 mm is attached to the tip side of the transfer pipe 3. Nozzle 9 of was connected.

In the film forming chamber 2, a vacuum pump 10 and a valve 1 are provided.
1 and the exhaust pipe 12, and the vacuum pump 10
The degree of vacuum in the film forming chamber 2 can be adjusted freely. In addition, the substrate 13 is horizontally placed in the film forming chamber 2 (direction of arrow X).
The substrate holding device 14 to be moved to was placed. Further, the tip portion of the transfer tube 3 connected to the particle generation chamber 1 was airtightly inserted into the film forming chamber 2.

The above-mentioned structure is not particularly different from the conventional apparatus for forming a fine particle film by the gas deposition method, but in the apparatus of the present invention, the fine particle generating chambers 1 and the film forming chambers 2 are arranged in tandem and the fine particle generating chambers are formed. The transport pipe 3 disposed between the evaporation source 7 in the chamber 1 and the substrate 13 in the film forming chamber 2 is formed into a straight line without any bend in the middle, and one end 15 of the transport pipe 3 is an evaporation source in the particle generation chamber 1. For example, they are arranged at an interval of 50 mm above 7 to serve as a carry-in port 15 for carrying the fine particles and the carrier gas, which are evaporated by the evaporation source 7 and are generated, to the film forming chamber 2 side. Further, the tip of the nozzle 9 at the tip of the transfer tube 3 is arranged at a predetermined distance from the substrate 13 in the film forming chamber 2, for example, 0.5 mm, and the fine particles together with the carrier gas are evaporated in the fine particle generating chamber 1. 7 allows the film to be directly conveyed to the substrate 13 in the film forming chamber 2 in a straight line.

Further, in the illustrated example, a discharge pipe 16 having an inner diameter of 25 mm is provided outside the carrier pipe 3 inserted in the particle generation chamber 1.
One end of which is concentrically arranged with the transfer pipe 3 in the fine particle generation chamber 1 in an airtight manner, and which serves as a discharge port 17 for the fine particles, and the other end of the discharge pipe 16 is disposed outside the fine particle generation chamber 1. It was connected to an exhaust system 18 such as an oil rotary pump via a valve 19.

Next, a specific example of forming a fine particle film will be described using the forming apparatus shown in FIG.

Embodiment First, the fine particle film material M is placed in the evaporation source 7 in the fine particle generating chamber 1.
After charging 20 g of Au as described above, helium gas was introduced from the gas supply source 5 into the fine particle production chamber 1 at a pressure of 2 atm while the flow rate was adjusted by the needle valve 6 so that the pressure was maintained. In addition, a substrate 13 made of alumina having a length of 70 mm and a width of 30 mm and a thickness of 1 mm is held in the substrate holding device 14 in the film forming chamber 2, and the surface of the substrate 13 and the tip of the nozzle 9 are 0.5 mm. After being held at the interval of, the substrate 13 was heated to a temperature of 200 ° C. by a substrate heating device (not shown).

Next, 400 W of electric power is applied to the basket-shaped evaporation source 7 by the evaporation source heating device 8 to heat the evaporation source 7 to melt and evaporate the fine particle film material M, and Au fine particles (average Particle size 0.1 μm) was produced.

Then, the vacuum pump 10 is operated to evacuate the film forming chamber 2 so that the pressure in the film forming chamber 2 is 0.3 To.
When maintained at rr, the Au fine particles generated in the fine particle generation chamber 1 due to the differential pressure between the fine particle generation chamber 1 and the film formation chamber 2 use the helium gas introduced into the fine particle generation chamber 1 as the carrier gas.
It is pressure-fed into the transfer tube 3 through the carry-in port 15 of the transfer tube 3, passes through the linear transfer tube 3 at a flow rate of 9 liters / min in a straight line, and is transferred into the film forming chamber 2. The nozzle 9 at the tip is preheated to the above temperature (200 ° C.), and the substrate holding device 14 moves at a speed of 7.5 mm in the moving direction (arrow X direction).
Au particles and a carrier gas were jetted onto the substrate 13 moving at a speed of / min to form an Au particle film F having a film thickness of 400 μm at a film deposition height rate of 100 μm / sec.

Immediately after the Au fine particle film F is formed on the substrate 13, the heating of the fine particle film material M by the evaporation source 7 and the transport of the fine particles by the carrier gas are stopped, and the exhaust system 1
The valve 19 of No. 8 was opened, and the Au fine particles remaining in the vicinity of the carry-in port 15 of the carrier pipe 3 were discharged from the discharge port 17 to the outside of the fine particle generation chamber 1.

When the Au fine particle film F formed on the substrate 13 was observed with a scanning electron microscope (magnification: 5,000 times), the particle size without agglomerates as shown in FIG. 2 was 0.1.
It was found that an Au fine particle film having a thickness of μm or less was formed. The adhesion of the Au fine particle film to the Ni film was examined and found to be 20 kgf / mm ² .

Comparative Example For comparison, the transfer pipe of the film forming apparatus was a transfer pipe 22 having a bent portion 21 bent once in a spiral shape (R: 60 mm), as shown in FIG. Other than the above, the forming apparatus shown in FIG.
A u fine particle film F ′ (see FIG. 4) was formed.

In the forming apparatus shown in FIG. 4, the symbol (2
The other reference numerals other than 1 and 22) are the same as those of the forming apparatus shown in FIG.

When the Au fine particle film F'formed on the substrate 13 was observed with a scanning electron microscope (magnification: 10,000 times), aggregates having a size of about 2 μm were recognized as shown in FIG. . Further, when the adhesion of the Au fine particle film to the Ni film was examined, it was 8 kgf / mm ² .

As is clear from FIGS. 2 and 5, in the embodiment of the present invention in which the fine particles and the carrier gas were conveyed straight, the Au fine particle film formed had no fine particle aggregation. In the comparative example in which the fine particles and the carrier gas were bent and conveyed during the conveyance, the formed Au fine particle film had aggregates of the fine particles. Therefore, it was confirmed that the formation of aggregates in the fine particle film formed on the substrate can be prevented by conveying the fine particles and the carrier gas in a straight line. In addition, the example of the present invention is
A fine particle film having improved adhesion to the film is formed, and the effect of greatly improving the adhesion of the fine particle film to the Ni film is exhibited by making the conveyance of the fine particles and the carrier gas straight.

In the forming apparatus shown in FIG. 1, a particulate discharge port 16 is provided in the vicinity of the carry-in port 15 of the carrier pipe 3, but instead of providing the discharge port, the position of the carry-in port 15 of the carrier pipe 3 and the evaporation source 7 are provided. A position adjusting device (not shown) such as a bellows or a spherical seal port for adjusting the relative position of the particle film is installed at either the carry-in port 15 of the carrier pipe 3 or the evaporation source 7. Immediately after the formation, the heating of the fine particle film material M by the evaporation source 7 and the conveyance of the fine particles by the carrier gas are stopped, and the position adjusting device is operated to move the conveyance pipe 3
Of the evaporation source 7 is moved from the position facing the evaporation port of the evaporation source 7 to change the relative position of the evaporation source 7 and the transfer port 15 of the carrier pipe 3, and the residual heat of the evaporation source 7 evaporates and generates. Therefore, it may be possible to prevent the fine particles remaining in the vicinity of the carry-in port 15 from being carried into the carrying pipe 3.

FIG. 3 shows another embodiment of the forming apparatus of the present invention. In the forming apparatus shown in FIG. 1, the fine particle producing chambers 1 and the film forming chambers 2 are arranged in tandem. This is an apparatus in which the forming chambers 2 are arranged in rows. Differences between the apparatus shown in FIG. 3 and the apparatus shown in FIG. 1 will be described.

The carry-in port 15 of the carrier pipe 3 which is airtightly inserted in the fine particle production chamber 1 is arranged above the evaporation source 7 in a lateral direction with respect to the evaporation source 7, and the laterally-carried carrier pipe 3 is linear as it is. The tip end of the transfer tube 3 is extended and inserted into the film forming chamber 2 in an airtight manner, and the tip of the nozzle 9 is attached to the particle forming chamber 1.
It was arranged with a predetermined distance, for example 0.5 mm, from the substrate 13 standing upright on the horizontal plane. Further, the discharge port 17 of the discharge pipe 16 is arranged above the evaporation source 7 and close to the carry-in port 15 of the carrier pipe 3. Since the other reference numerals are the same as those of the forming apparatus shown in FIG. 1, the description thereof will be omitted.

When the apparatus of FIG. 3 is contrasted with the apparatus of FIG. 1, the fine particle production chamber 1 remains as it is, and the film forming chamber 2 and the transfer tube 3 are in a state of lying sideways with respect to the fine particle production chamber. Also,
The operation and effects of the forming apparatus shown in FIG. 3 are the same as those of the forming apparatus shown in FIG.

In the forming apparatus shown in FIG. 1, the particle generation chamber 1
The film forming chambers 2 and the film forming chambers 2 are arranged in tandem, but the present invention is not limited to this, and the transfer pipe 3 connecting the evaporation source 7 in the particle generation chamber 1 and the substrate 13 in the film forming chamber 2 is linear. It suffices that the fine particle generation chambers 1 and the film formation chambers 2 be arranged side by side in the laid-down state as they are arranged in a column. Further, in the forming apparatus shown in FIG. 3, the particle generation chamber 1 and the film formation chamber 2 are arranged in a row, but the present invention is not limited to this, and the evaporation source 7 and the film formation chamber in the particle generation chamber 1 are not limited to this. It suffices that the transfer tube 3 connecting the substrate 13 in 2 can be linearly arranged, and the fine particle generation chambers 1 and the film formation chambers 2 may be vertically arranged in a horizontal arrangement.

[0029]

According to the method of forming a fine particle film by the gas deposition method of the present invention, the fine particles and the carrier gas are conveyed straight between the evaporation source and the substrate by a straight conveying pipe which does not bend. Since it is performed in a state, since the gas flow is not disturbed during transportation, agglomeration due to collision of fine particles does not occur in the transportation process, and the adhesion with the substrate is good,
There is an effect that it is possible to form a fine particle film having a high density without agglomerates on a substrate very easily.

When the apparatus for forming a fine particle film by the gas deposition method of the present invention is used, the transfer tube for transferring the fine particles and the carrier gas is formed in a straight line without bending between the evaporation source and the substrate. Therefore, it is possible to convey the fine particles and the carrier gas in a straight line state, the adhesion force with the substrate is good, and it is possible to extremely easily form the fine particle film on the substrate, which has an increased density without aggregation. There is an effect that a forming device can be provided.

Further, by providing an adjusting mechanism for adjusting the relative position between the evaporation source and the carry-in port of the carrier pipe, it can be adjusted to a position where the concentration of particles produced by evaporation is large, and a sufficient deposition rate can be secured.

If a discharge port for discharging fine particles is provided in the vicinity of the carry-in port of the transfer pipe, excess particles not used for film formation can be excluded, and generation of aggregates due to convection in the fine particle generation chamber can be excluded. .

[Brief description of drawings]

FIG. 1 is an explanatory diagram of one embodiment of the device of the present invention,

FIG. 2 is a drawing-substituting photograph showing the surface condition of a fine particle film formed on a substrate in one embodiment of the method of the present invention,

FIG. 3 is an explanatory diagram of another embodiment of the device of the present invention,

FIG. 4 is an explanatory diagram of a forming apparatus used for comparison with the method of the present invention;

5 is a photograph as a substitute for a drawing showing a surface state of a fine particle film formed on a substrate by the forming apparatus shown in FIG.

FIG. 6 is an explanatory diagram of a conventional forming apparatus.

[Explanation of symbols]

1 fine particle generating chamber, 2 film forming chamber, 3 carrier pipe, 7 evaporation source, 9 nozzle, 1
3 substrates, 15 carry-in port, 17 discharge port, F
Fine particle film, M Fine particle film material.

Claims (4)

[Claims] 1. A gas deposition method in which fine particles are transported together with a carrier gas in a transport tube and the fine particles are formed on a substrate by jetting the fine particles from a nozzle at the tip of the transport tube.
A method of forming a fine particle film by a gas deposition method, characterized in that fine particles and carrier gas are conveyed between a vaporization source and a substrate by a linear conveying pipe. 2. An evaporation source of the fine particle film material, a substrate, a carrier pipe for carrying the fine particles of the fine particle film material together with a carrier gas, and a nozzle provided at the tip of the carrier pipe for injecting the fine particles and the carrier gas onto the substrate. In the apparatus for forming a fine particle film by the gas deposition method, the transfer tube is a transfer tube formed in a straight line without bending between the evaporation source and the substrate. Membrane forming device. 3. The gas deposition method according to claim 2, further comprising an adjusting mechanism for adjusting the relative positions of the evaporation source, the fine particles in the carrier pipe and the carrier gas inlet. Device for forming fine particle film. 4. An apparatus for forming a fine particle film by the gas deposition method according to claim 2, wherein an outlet for discharging the fine particles is provided in the vicinity of the inlet for the fine particles and the carrier gas of the carrier pipe. .