JPH07321040A - Metallic compound container - Google Patents

Abstract

PURPOSE:To stabilize the feeding of a metallic compound gas by a method wherein a carrier gas inlet is arranged at a position not making a direct contact with the metallic compound stored in a reservoir for preventing the sublimation rate from being made uneven on the metallic compound. CONSTITUTION:A carrier gas inlet 2 leading in a carrier gas 11 and a metallic compound gas exhaust port 7 are arranged to be separated from each other near both ends on the surface of a reservoir 1. At this time, a carrier gas piping 5 following after the carrier gas inlet 2 is arranged in the reservoir 1 so that the carrier gas 11 led in from the inlet 2 may be once led to the lower part of the reservoir 1, but later blown upward in the reservoir 1. Accordingly, the carrier gas 11 blown out of the piping 5 is not brought into direct contact with the metallic compound 10 stored in the reservoir 1.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a metal compound container for supplying a metal compound gas having a stable concentration to an apparatus for forming a metal thin film by a CVD method.

[0002]

2. Description of the Related Art A conventional metal compound container is shown in FIG.
Will be described with reference to.

In the reservoir 1, powdery metal compound 1
0 is stored, and the carrier gas 11 is blown out from the carrier gas introduction port 2 provided on the upper surface of the reservoir 1. Next, the metal compound 10 stored in the reservoir 1 is sublimated into the carrier gas 11 by heating the reservoir 1 by the heater 4, and the sublimated metal compound gas 12 is an upper surface of the reservoir 1. It is taken out from the metal compound gas discharge port 7 provided in the.

However, in this conventional metal compound storage container, the carrier gas 11 flows as shown by C in FIG.
Since the metal compound 10 directly below the carrier gas inlet 2 directly hits and the metal compound 10 stored at that position is sublimated excessively with respect to the surrounding metal compound 10, the carrier gas is changed over time. The metal compound 10 immediately below the inlet 2 rapidly decreases (see D in the figure).
As a result, the concentration of the discharged metal compound gas 12 shows a high concentration value immediately after the metal compound 10 is stored in the reservoir 1, and thereafter, the metal compound 10 directly below the carrier gas inlet 2 decreases. However, there is a problem in that the density gradually decreases as the temperature increases.

Further, the metal compound gas 12 discharged
Is a mixture of the sublimated metal compound gas 12 and the introduced carrier gas 11 in the reservoir 1.
In order to keep the mixing ratio constant, it is necessary to stir the mixture, but without stirring, the mixing ratio of the metal compound gas 12 and the carrier gas 11 in the mixed gas discharged from the reservoir 1 is not stable. Therefore, the supply amount of the metal compound gas 12 to the CVD device is not stable, and C
Since the processing conditions of the VD apparatus are unstable, there is also a problem in that the quality and thickness of the metal thin film produced by this CVD apparatus are affected.

With respect to such problems, a technique relating to a metal compound storage container for the purpose of stable supply of raw materials is disclosed in JP-A-64-64314 and JP-A-3-2.
It is disclosed in Japanese Patent Publication No. 27011.

The technique disclosed in Japanese Patent Laid-Open No. 64-64314 is a sublimator for sublimating an organic metal which is solid at room temperature by using a carrier gas, and has a mesh shape provided in a closed container. By adhering the organic metal to the wire net and introducing the carrier gas into it, the contact area between the carrier gas and the organic metal increases, and therefore, the organic metal stably sublimes in the carrier gas at saturated vapor pressure. , A stable amount of organic metal gas is taken out without being affected by the remaining amount of organic metal.

The technique disclosed in Japanese Patent Laid-Open No. 3-227011 is a device for stably supplying a vapor of a solid material for a long time to a crystal growth device such as a semiconductor laser.
A pipe for introducing a carrier gas into the container is spirally formed of a shape memory alloy, and the organometallic compound gas is first discharged in a state where the pipe is embedded in the organic metal packed in the container. Next, when the concentration of the discharged organometallic compound gas is nonuniform, the temperature of the container is raised to change the shape of the pipe made of the shape memory alloy, and the container is packed. Stir the organometallic. Thereby, the concentration of the discharged organometallic compound gas is returned to the original state.

[0009]

DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention
The technique disclosed in Japanese Patent No. 4314 has a problem in that the metal compound attached to the mesh and the introduced carrier gas have a large contact area, so that the metal compound is consumed significantly.

Furthermore, since it is necessary to attach a mass of the metal compound to the mesh-like wire net, it takes a lot of time and labor for processing, and the structure of the metal compound storage container itself becomes complicated.

Further, in the technique disclosed in Japanese Patent Application Laid-Open No. 3-227011, the shape of the pipe made of the shape memory alloy is changed when the concentration of the metal compound gas discharged from the reservoir becomes low. Therefore, in order to stir the metal compound in the reservoir, it is necessary to provide a means for measuring the concentration of the discharged metal compound gas, and it is difficult to know the timing of actually stirring the metal compound. There was a problem.

Further, there is a problem that it is very difficult to return the concentration of the discharged metal compound gas to the original value by changing the shape of the pipe even if the metal compound is stirred. .

[0013]

In order to solve the above problems, a metal compound storage container according to the present invention comprises a reservoir in which a metal compound is stored, and a carrier gas inlet for introducing a carrier gas into the reservoir. A metal compound storage container provided with a heater for heating the reservoir for sublimating the metal compound, and a metal compound gas discharge port for discharging a mixed gas of the sublimated metal compound and the carrier gas from the reservoir The carrier gas introduction port is arranged at a position where the introduced carrier gas does not directly hit the metal compound stored in the reservoir.

[0014]

Next, a first embodiment of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a diagram showing the configuration of the first embodiment, in which a carrier gas inlet 2 for introducing a carrier gas 11 and a metal compound gas outlet for discharging a metal compound gas 12 are provided on the upper surface of a reservoir 1. 7 are provided separately from each other near both ends, and by opening and closing the valves 3 and 8, the carrier gas 11 is introduced or the metal compound gas 12 is introduced.
Is discharged. A powdery metal compound 10 is stored in the reservoir 1.

The carrier gas pipe 5 is provided in the reservoir 1 following the carrier gas inlet 2, and the carrier gas 11 introduced from the carrier gas inlet 2 is provided.
Is once guided to the lower part of the reservoir 1, and thereafter, the carrier gas 11 is arranged to be blown upward in the reservoir 1. That is, the carrier gas 11 blown out from the pipe 5 is configured so as not to directly hit the metal compound 10 stored in the reservoir 1.

The heater 4 is provided around the reservoir 1 and heats the reservoir 1 so that the temperature in the reservoir 1 is equal to or higher than the sublimation temperature of the metal compound 10.

The temperature sensor 9 measures the temperature in the reservoir 1 and detects a change in the concentration of the metal compound gas 12 discharged from the reservoir 1, and based on the detection result, the heater 4 is operated by the heater 1. Control the heating of.

Next, the operation of this embodiment will be described with reference to FIG.

First, the valve 3 is opened to introduce the carrier gas 11 from the carrier gas inlet 2. At this time, since the reservoir 1 is heated by the heater 4, the metal compound 10 stored in the reservoir 1 is sublimated.

The carrier gas 11 introduced from the carrier gas inlet 2 is guided by the carrier gas pipe 5 and blown into the reservoir 1 from the carrier gas outlet 6 facing upward in the reservoir 1. Here, since the carrier gas blowing port 6 faces upward in the reservoir 1 and the carrier gas 11 does not directly hit the metal compound 10, the sublimation rate of a specific portion on the metal compound 10 Does not increase, and a uniform sublimation rate can be maintained. In addition, by increasing the position of the carrier gas outlet 6, it is possible to increase the amount of the metal compound 10 that can be stored.

The carrier gas 11 blown into the reservoir 1 is mixed with the sublimated metal compound 10. Here, the carrier gas 11 is blown out from the carrier gas outlet 6 and then flows so as to stir in the reservoir 1 as shown by A in the figure, so that the concentration of the mixed metal compound gas 12 is increased. It becomes uniform.

The metal compound gas 12 having a uniform concentration is
The gas is discharged from the metal compound gas discharge port 7 with the valve 8 opened.

Here, the temperature inside the reservoir 1 is measured by the temperature sensor 9, the change in the concentration of the metal compound gas 12 due to the change in the sublimation amount of the metal compound 10 is detected, and the reservoir by the heater 4 is detected. 1 heating is controlled.

Next, a second embodiment of the present invention will be described with reference to the drawings.

FIG. 2 is a diagram showing the configuration of the second embodiment, and the description of the configuration similar to that of the first embodiment will be omitted.

In FIG. 2, the carrier gas inlet 2 and the metal compound gas outlet 7 are provided separately on the side surface of the reservoir 1. However, the carrier gas introduction port 2 for introducing the carrier gas 11 must be installed below, and the metal compound gas discharge port 7 for discharging the metal compound gas 12 must be installed above. Must be installed at a position higher than the upper surface of the metal compound 10 stored in the reservoir 1.

That is, in the second embodiment, as compared with the above-described first embodiment, the installation positions of the carrier gas inlet 2 and the metal compound gas outlet 7 are changed so that the carrier gas pipe is installed. The difference is that it is unnecessary.

Next, the operation of the second embodiment will be described with reference to FIG.

First, the carrier gas 11 is blown into the reservoir 1 through the carrier gas inlet 2. Here, the metal compound 10 in the reservoir 1 is heated by the heater 4.
Is sublimated.

The carrier gas 11 blown into the reservoir 1 is mixed with the sublimated metal compound 10, and further,
After flowing so as to stir in the reservoir 1 as shown by B in the figure, it is discharged from the metal compound gas discharge port 7.

The installation positions of the carrier gas introduction port 2 and the metal compound discharge port 7 in the metal compound storage container of the present invention are not limited to the above-mentioned embodiments, and the carrier gas 11 blown out is stored in the reservoir 1. Metal compound 10
The point where the carrier gas 11 in the reservoir 1 does not directly hit and the point where the carrier gas 11 in the reservoir 1 flows so as to stir in the reservoir 1.
The carrier gas inlet 2 and the metal compound gas outlet 7 may be arranged so as to satisfy the four conditions.

In addition, since the concentration of the metal compound gas 12 discharged from the metal compound storage container of each of the above-described embodiments is stable, the present invention can focus laser light emitted from a laser oscillator on a sample. Irradiation causes thermal decomposition of the metal compound gas blown to the laser light irradiation point,
When used in a laser CVD apparatus for depositing a metal thin film on the surface of the sample, stable and highly accurate laser CVD can be performed.

[0034]

As described above, in the metal compound storage container of the present invention, by arranging the carrier gas inlet so that the introduced carrier gas does not directly hit the metal compound, the sublimation rate on the metal compound is increased. To prevent non-uniformity and realize stable supply of metal compound gas.

Further, the carrier gas is supplied by arranging the carrier gas inlet and the metal compound gas outlet so that the carrier gas introduced into the reservoir flows together with the sublimated metal compound so as to stir in the reservoir. It is possible to stabilize the concentration of the metal compound gas.

[Brief description of drawings]

FIG. 1 is a sectional view showing a configuration of a first embodiment of the present invention.

FIG. 2 is a sectional view showing the configuration of a second embodiment of the present invention.

FIG. 3 is a cross-sectional view showing the configuration of a conventional metal compound storage container.

[Explanation of symbols]

 1 Reservoir 2 Carrier Gas Inlet 3 Valve 4 Heater 5 Carrier Gas Pipe 6 Carrier Gas Outlet 7 Metal Compound Gas Outlet 8 Valve 9 Temperature Sensor 10 Metal Compound 11 Carrier Gas 12 Metal Compound Gas

Claims (2)

[Claims] 1. A reservoir storing a metal compound, a carrier gas inlet for introducing a carrier gas into the reservoir, a heater for heating the reservoir to sublimate the metal compound, and the sublimated metal. In a metal compound storage container provided with a metal compound gas outlet for discharging a mixed gas of a compound and the carrier gas from the inside of the reservoir, the introduced carrier gas is placed at a position where it does not directly hit the metal compound stored in the reservoir. A metal compound storage container having a carrier gas introduction port. 2. A reservoir storing a metal compound, a carrier gas inlet for introducing a carrier gas into the reservoir, a heater for heating the reservoir to sublimate the metal compound, and the sublimated metal. In a metal compound storage container provided with a metal compound gas outlet for discharging a mixed gas of a compound and the carrier gas from the inside of the reservoir, the carrier gas is introduced so that the introduced carrier gas stirs the metal compound gas inside the reservoir. A metal compound storage container having an inlet and the metal compound gas outlet.