JPH03131018A - Supply of solid organic metal material and container for supply - Google Patents

Abstract

PURPOSE:To enable a solid organic metal material to be supplied to a reaction pipe stably by housing a number of short pipes where a solid organic metal material is adhered to the inner wall within a container for supplying the solid organic metal material and by enabling a carrier gas which is supplied to the container for supply to pass through a hollow part of each hollow short pipe. CONSTITUTION:When a carrier gas CG is supplied to the hole of a supply part 4 or into a container for supply 1, the gas CG flows to each hollow short pipe 13, 13... which are housed within the container for supply 1 and then are sent to a reaction pipe by a pipe which is connected to a joint 6. When the carrier gas CG passes the inside of the hollow part in each hollow short pipe 13, 13... which are housed within the container for supply 1, it flows being in contact with the surface of organic metal materials 14, 14... which are adhered to an inner wall of each hollow short pipe 13, 13... and the carrier gas CG with is sent from the container for supply 1 to the reaction pipe can carry system pressure of the solid organic metal material corresponding to the saturation steam pressure of the solid organic metal material at the temperature within the container for supply 1 toward the reaction pipe.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a solid organometallic material supply method and a supply container.

(Prior Art) When producing a compound semiconductor or a superconducting thin film by MOCVD using a solid organometallic material as a raw material, the solid organometallic material is stored in a supply container.

A method for supplying a solid organometallic material has been tried in the past, in which the vapor pressure of the solid organometallic material carried by a carrier gas supplied into a container for supplying the solid organometallic material is supplied to a reaction tube. It's coming.

3 to 6 are diagrams for explaining a conventional method for supplying solid organic metal materials. In FIG. 3, 1 is a supply container made of stainless steel, for example.

Inside this supply container 1 is a mass of solid organometallic material 5.5.
5... is stored.

Reference numeral 3 denotes an introduction pipe for introducing carrier gas CG from the outside of the supply container 1 into the inside of the supply container 1, and this introduction pipe 3 is in a state where high airtightness can be maintained between the supply container 1 and the carrier gas CG. It is inserted into the supply container 1.

A carrier gas C (not shown) is connected to the connection part 2 provided at the end of the introduction pipe 3 outside the supply container 1.
The piping from the G supply source is connected.

Further, a carrier gas supply section 4 is provided at the end of the introduction pipe 3 inside the supply container 1 .

Reference numeral 6 denotes a connection part for connecting a pipe for supplying the carrier gas discharged from the supply container 1 and the vapor pressure of the solid organometallic material carried by the carrier gas to a reaction tube (not shown). .

In FIG. 3, an inlet pipe 3 is connected to a connection part 2 from a supply source of carrier gas CG (not shown).
The carrier gas introduced into the supply container 1 by
The carrier gas CG is supplied into the supply container 1 from a large number of holes in the carrier gas supply section 4, and the carrier gas CG is supplied to the solid organometallic material lumps 5, 5, 5, . . . stored in the supply container 1.
It is sent to a reaction tube (not shown) by a pipe that passes through the space and is connected to the connection part 6.

FIG. 4 shows that nets 7 to 10 are stretched inside the supply container 1, and a mass of solid organometallic material 5 is placed on the nets 7 to 10.
This is a conventional example in which the flow of the carrier gas is forcibly made uniform by the nets 7 to 10 so that the lump 5 of the solid organometallic material can come into contact with the carrier gas CG over a large area, and FIG. As shown by the enlarged cross-sectional view in Figure 6,
Conventional example in which a solid organometallic material 12 is attached to the surface of a sphere 11゜11... and is housed in a supply container 1 so that a carrier gas CG can come into contact with the solid organometallic material over a large area. In the conventional example shown in FIGS. 4 and 5, as in the case of the conventional example explained with reference to FIG. The carrier gas introduced into the supply container 1 through the introduction pipe 3 connected to the carrier gas supply section 2 is supplied into the supply container 1 from a large number of holes in the carrier gas supply section 4, and the carrier gas CG is In the case of the conventional example shown in FIG. 4, lumps of solid organometallic material 5, 5.
... and is sent to a reaction tube (not shown) by a pipe connected to the connection part 6, and in the case of the conventional example shown in FIG. 5, it is stored in the supply container 1. A reaction (not shown) is carried out by a pipe that passes through the solid organometallic material 12 attached to the surface of each sphere 11, 11... while in contact with the surface and is connected to the connection part 6. sent to the tube.

In any of the conventional solid organometallic material supply methods described above with reference to FIGS. 3 to 6, the interior of the supply container 1 is It is expected that the vapor pressure of the solid organometallic material corresponding to the saturated vapor pressure of the solid organometallic material at the temperature of 200 nm will be carried toward the reaction tube by the carrier gas.

(Problems to be Solved by the Invention) Including the solid organic metal material supply method explained with reference to FIGS. 3 to 6, the solid organic metal material is stored in a supply container, and the solid organic metal material is In the solid organometallic material supply method in which the vapor pressure of the solid organometallic material transported by the carrier gas supplied into the metal material supply container is supplied to the reaction tube, the solid organometallic material stored in the supply container is Assuming that the solid organometallic material is saturated at the saturated vapor pressure at the temperature in the supply container, wRWI of the amount of solid organometallic material supplied to the reaction tube is performed by adjusting the flow rate of the carrier gas. Since the carrier gas that has passed through contact with the solid organometallic material contained in the supply container is a solid organic material that corresponds to the saturated vapor pressure of the solid organometallic material at the temperature in the supply container It is assumed that the vapor pressure of the metal material is being transported.

In order for the above premise to hold, it is necessary to increase the contact area between the carrier gas and the surface of the solid organometallic material, and to change the state from a state in which there is a large amount of solid organometallic material stored in the supply container to a solid state. It is necessary that the remaining amount of the organometallic material remains constant even when the remaining amount is small.

However, in the case of the conventional solid organometallic material supply method explained with reference to FIG. 3, about 40% to 50% of the solid organometallic material stored in the supply container is used. In this case, it was observed that the supply state of the solid organometallic material supplied from the supply container to the reaction tube became unstable, and a phenomenon occurred in which the composition of the crystals produced in one reaction tube varied as the crystals grew.

It is thought that the above phenomenon is caused by the carrier gas passage being fixed, creating a large carrier gas passage, and not all of the carrier gas necessarily coming into contact with the surface of the solid organometallic material. 4 and 5 as a means to solve the problem.

Although a method for supplying a solid organometallic material as described with reference to FIG. 6 has been proposed, even this method cannot completely prevent the above-mentioned phenomenon from occurring.

(Means for Solving the Problems) The present invention stores a large number of short hollow tubes, each of which has a solid organometallic material adhered to its inner wall, in a container for supplying the solid organometallic material. A method for supplying a solid organometallic material in which the vapor pressure of the solid organometallic material carried by a carrier gas supplied in a supply container can be supplied to a reaction tube, and a solid organometallic material attached to an inner wall thereof. A certain number of hollow short tubes are housed in a vessel, and a means for discharging and supplying a carrier gas into the vessel, and a vapor pressure portion of a solid organometallic material carried by the carrier gas from inside the vessel is supplied to a reaction tube. and means for supplying solid organometallic material.

(Function) A large number of short hollow tubes each having a solid organometallic material adhered to the inner wall thereof are housed in a container for supplying the solid organometallic material, and a carrier gas is supplied into the container for supplying the solid organometallic material. is made to flow through the hollow portion of each of the hollow short tubes described above.

As a result, the carrier gas always flows in contact with the solid organometallic material attached to the inner wall of the short hollow tube, so that the solid organometallic material can always be stably supplied to the reaction tube.

(Example) Hereinafter, specific contents of the solid organic metal material supply method and supply container of the present invention will be explained in detail with reference to the accompanying drawings. FIGS. 1 and 2 are perspective views for explaining the solid organic metal material supply method and supply container of the present invention.

In FIG. 1, reference numeral 1 denotes a supply container made of stainless steel, for example, and a solid organometallic material 14 such as trimethylindium (TMI) is provided on the inner wall of the supply container 1.
A large number of short hollow tubes 13, 13, .

Reference numeral 3 denotes an introduction pipe for introducing carrier gas CG from the outside of the supply container 1 into the inside of the supply container 1, and this introduction pipe 3 is in a state where high airtightness can be maintained between the supply container 1 and the carrier gas CG. It is inserted into the supply container 1. A connection part 2 provided at the end of the introduction pipe 3 outside the supply container 1
A pipe from a carrier gas CG supply source (not shown) is connected to the carrier gas CG, and a carrier gas supply section 4 is provided at the end of the introduction pipe 3 inside the supply container 1 .

Reference numeral 6 denotes a connection part for connecting a pipe for supplying the carrier gas discharged from the supply container 1 and the vapor pressure of the solid organometallic material carried by the carrier gas to a reaction tube (not shown). .

In FIG. 1, an inlet pipe 3 to which a pipe from a carrier gas CG supply source (not shown) is connected to a connecting part 2.
When the carrier gas CG, such as high-purity hydrogen gas, introduced into the supply container 1 by the carrier gas is supplied into the supply container 1 from the numerous holes of the carrier gas supply section 4,
After the carrier gas CG flows through the hollow portions of the respective hollow short pipes 13, 13... housed in the supply container 1, a reaction (not shown) is carried out by piping connected to the connection part 6. sent to the tube.

By the way, the carrier gas CG described above is supplied to the supply container 1.
When passing through the hollow portion of each hollow short tube 13, 13... stored in the interior, it is necessary to pass through each hollow short tube as shown in the enlarged example in FIG. 13,13...
An organometallic material attached to the inner wall of 14.14.
The carrier gas CG sent from the supply container 1 to the reaction tube is a solid organic material whose temperature corresponds to the saturated vapor pressure of the solid organometallic material at the temperature inside the supply container 1. This means that the vapor pressure of the metal material can be transported toward the reaction tube.

The short hollow tube mentioned above may be made of, for example, quartz or stainless steel, and the solid organic metal material 14 is adhered to its inner wall. Further, the above-mentioned hollow short tube may have a circular, triangular, polygonal, or other arbitrary cross-sectional shape.

(Effects of the Invention) As is clear from the above detailed explanation, in the solid organometallic material supplying method of the present invention, a large number of hollow short tubes having the solid organometallic material attached to the inner wall are connected to the solid organometallic material. The carrier gas stored in the supply container of the solid organometallic material and supplied into the supply container of the solid organometallic material always flows through the hollow portion of each of the hollow short tubes. Since the carrier gas flows in contact with the solid organometallic material attached to the inner wall of the hollow short tube over a wide area, there is always a flow from the supply container of the solid organometallic material to the reaction tube. Since a solid organic metal material can be stably supplied, the above-mentioned conventional problems can be satisfactorily solved according to the present invention.

[Brief explanation of the drawing]

1 and 2 are perspective views for explaining the solid organic metal material supply method and supply container of the present invention, and FIGS. 3 to 6 are side sectional views for explaining a conventional example. DESCRIPTION OF SYMBOLS 1... Supply container, 2, 6... Connection part, 3... Introducing pipe, 4... Carrier gas supply part, 5, 12, 14
...Solid organometallic material, 7-10...Mesh, 13...
・Hollow short tube.

Claims (1)

[Claims] 1. A number of short hollow tubes having a solid organometallic material adhered to the inner wall thereof are housed in a container for supplying the solid organometallic material,
2. A method for supplying a solid organometallic material in which the vapor pressure of the solid organometallic material carried by the carrier gas supplied into the container for supplying the solid organometallic material can be supplied to the reaction tube. A number of hollow short tubes having solid organic metal materials attached to the inner walls are housed in the vessel, and a means for releasing and supplying a carrier gas into the vessel, and a solid organic metal material transported from the vessel by the carrier gas. 2. A container for supplying a solid organometallic material, comprising means for supplying a vapor pressure of 3. 4. A container for supplying solid organic metal material according to claim 2, wherein the container for supplying solid organic metal material is made of stainless steel. 5. A container for supplying a solid organometallic material according to claim 2, wherein the short hollow tube having the solid organometallic material adhered to the inner wall is made of quartz. 3. The solid organometallic material supply container according to claim 2, wherein the short hollow tube having the solid organometallic material adhered to its inner wall is made of stainless steel.