JPH06232048A - Device for vaporizing and supplying organometallic compound - Google Patents

Abstract

PURPOSE:To maintain a vaporizing container at a vaporizing temperature containing less errors as a whole by arranging a saucer to be filled with the powder of an organometallic compound in the container and forming carrier gas flowing-in and flowing-out holes through the side wall of the container. CONSTITUTION:A vaporizing container 11 is dipped in oil 9 contained in an oil bath 8 constituting a constant-temperature bath. The flowing-out hole 12 of a carrier gas 14 and starting gaseous material to a CVD reaction device 15 and the flowing-in hole of the carrier gas 14 to container 11 are interposed to each other. The saucer 16 to be filled with an organometallic compound 4 which is used as the raw material has such a shape that the surface area of the saucer 16 does not change even when the amount of the compound 4 decreases by evaporation. The holes 10 and 12 are formed through the side wall of the container 11 at heights higher than the saucer 16 and interposed to each other. Therefore, thin films which always have the same characteristic values under the same condition can be obtained.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is applied to the production of thin films of compound semiconductors, dielectrics, superconductors, magnetic materials, etc. by a vapor phase growth method (MO-CVD method) using an organometallic compound as a raw material. The present invention relates to an apparatus for vaporizing and supplying an organometallic compound which is a solid raw material used as the raw material.

[0002]

2. Description of the Related Art With the recent miniaturization, weight reduction and high performance of electronic devices, many attempts have been made to thin magnetic materials and dielectric materials, and various film forming methods have been studied. . The MO-CVD method using an organometallic compound as a raw material, which is one of the film forming methods, is industrially excellent because a large-area thin film can be obtained at a high speed under a relatively low degree of vacuum. Another film forming method.

In the MO-CVD method, as a method of vaporizing a solid organometallic compound which is a raw material and introducing it into a CVD reactor, a powder of a solid organometallic compound which is a solid raw material has been conventionally put in a quartz boat. It is a general method to place in a quartz tube under reduced pressure, vaporize by heating with an electric resistance heater from the outside of the quartz tube, and introduce with a carrier gas whose flow rate is controlled.

FIG. 2 is a block diagram of a conventional vaporizing and supplying apparatus according to this method. In the figure, 1 is a mass flow controller (MFC) for controlling the flow rate of the carrier gas 14, 2
Is a quartz tube, 3 is a quartz boat, 4 is a raw material organometallic compound, 5 is a thermocouple, 6 is an electric resistance heater, and 7 is a temperature controller for controlling the vaporization temperature.

This device is used as follows. First, a predetermined amount of the organometallic compound 4 as a raw material is put on the quartz boat 3. This is put in the quartz tube 2 and decompressed by a vacuum pump. The quartz tube 2 and the entire quartz boat 3 in the quartz tube 2 are heated by an electric resistance heater 6 and kept at a predetermined temperature by a thermocouple 5 and a temperature controller 7.
Vaporize. A carrier gas 14 whose flow rate is controlled by the mass flow controller 1 is flown into the quartz tube 2 and introduced into the CVD reactor 15 together with the vaporized source gas. Such a vaporization supply device for a CVD reactor is disclosed, for example, in Journal of Material Science (1989), pages 3549 to 3552.

However, in the case where such a vaporization supply device is manufactured and film formation is performed, there is a problem that the film thickness and various physical property values vary even if the raw material is vaporized and formed under the same conditions. This is because the electric resistance heater 6 located outside the quartz tube 2 is used to heat the organometallic compound 4, so that the vaporization temperature of the raw material varies and the raw material on the quartz boat 3 gradually decreases. It is conceivable that the area in contact with the carrier gas 14 changes as the process proceeds and the amount of vaporization of the raw material changes.

In order to solve this problem, therefore, a cylindrical vaporization container is directly filled with powder of an organometallic compound,
A vaporization supply device has been proposed in which this vaporization container is immersed in an oil bath for heating, a carrier gas whose flow rate is controlled is made to flow from above, and is introduced into the CVD reaction device together with the source gas from above again.

FIG. 3 is a block diagram of a vaporization and supply device according to this method. In the figure, 8 is an oil bath, 9 is oil, 10 is an inlet for carrier gas 14, 11 is a vaporization container, 12 is an outlet for carrier gas 14 and source gas, and 13 is a lid for the vaporization container 11. In addition, the same members as those in FIG. 2 are denoted by the same reference numerals, and the description thereof will be omitted.

This device is used as follows. First, the raw material organometallic compound 4 is filled in the vaporization container 11. A lid 13 having an inflow hole 10 and an outflow hole 12 is attached to the vaporization container 11 and submerged in the oil 9 in the oil bath 8. Vaporization container 11
Is heated by an oil bath 8 via oil 9, and is kept at a predetermined temperature by a thermocouple 5 and a temperature controller 7 installed immediately below the vaporization container 11. A carrier gas 14 whose flow rate is controlled by the mass flow controller 1 is caused to flow into the vaporization container 11 through the inflow hole 10 and is introduced into the CVD reaction device 15 through the outflow hole 12 together with the vaporized raw material gas. CV like this
The vaporization supply device of the D reactor is disclosed in, for example, Journal of Applied Magnetics of Japan (1988), pages 339 to 342.

[0010]

However, when a film is formed by using the vaporization supply device as shown in FIG. 3, even if the raw material is vaporized under the same conditions to form the film, the film thickness and various types of film are still generated. There was a problem that the physical property values were slightly different. The reason for this is that the carrier gas 14 for supplying the vaporized source gas of the organometallic compound 4 to the CVD reactor 15 flows in through the inflow hole 10 above the vaporization vessel, and flows out again through the outflow hole 12 together with the source gas. Therefore, turbulence occurs in the gas flow in the vaporization container 11, and it is not possible to supply all of the vaporized raw material gas to the CVD reactor 15. Also, the heating of the organometallic compound is performed using the oil bath 8. By doing so, the vaporization temperature with very few errors can be set.
It is considered that the temperature gradient in the vaporization container hinders the stable supply of the raw material gas because the upper part of the is in the atmosphere.

An object of the present invention is to solve the above-mentioned conventional problems and to provide a vaporization and supply device of an organometallic compound which can always obtain a thin film having the same characteristic value under the same conditions.

[0012]

The apparatus for vaporizing and supplying an organometallic compound according to the present invention has a vaporization container and a constant temperature bath for containing the vaporization container, and the vaporization container is filled with the powder of the organometallic compound. And a carrier gas inflow hole and a carrier gas outflow hole are arranged in the side wall of the vaporization container.

The carrier gas inflow hole and outflow hole in the vaporizing and supplying apparatus for the organometallic compound are located on the side wall above the dish filled with the organometallic compound powder placed in the vaporizing vessel, and face each other. By being arranged, the carrier gas is configured to flow parallel to the surface of the powder of the organometallic compound.

Further, in the dish filled with the powder of the organometallic compound in the vaporization container, the surface area of the surface of the powder of the organometallic compound filled in the dish is not affected by the vaporization of the powder of the organometallic compound. , Having a shape that is always constant.

Further, the constant temperature bath is composed of an oil bath, and the vaporization temperature of the powder of the organometallic compound is controlled by submerging the entire vaporization vessel in the oil bath and controlling the temperature of the oil to heat the entire vaporization vessel. It is designed to be controlled.

[0016]

According to the present invention, the powder of the organometallic compound as a raw material is filled in a dish whose surface area is always constant regardless of the decrease in the surface area due to the vaporization of the raw material, and the dish is placed. By supplying the source gas to the CVD reactor by flowing the carrier gas in the vaporization container in parallel with the surface of the powder of the organometallic compound, it is possible to always maintain a stable supply amount of the source gas. Furthermore, for heating the organometallic compound as a raw material, by putting the entire vaporization container in a thermostatic bath (for example, an oil bath), the vaporization supply device for the organometallic compound that can maintain the vaporization temperature of the entire vaporization container with very few errors Is provided.

Therefore, by using the apparatus for vaporizing and supplying an organometallic compound of the present invention, it is possible to obtain a thin film having the same characteristic values under the same vaporization conditions. In addition, since the plate for filling the organometallic compound as a raw material is separately provided, it has an advantage that it is easy to replace the raw material and clean the inside of the vaporization container.

[0018]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An organometallic compound vaporizing and supplying apparatus according to an embodiment of the present invention will be described below with reference to the drawings.

FIG. 1 is a block diagram of an apparatus for vaporizing and supplying an organometallic compound according to an embodiment of the present invention.

As shown in FIG. 1, the constitution of this embodiment is characterized in that the constant temperature bath is constituted by an oil bath 8, and a vaporization container 11 is arranged in the oil 9 in the oil bath 8. Outflow hole 12 for carrier gas 14 and source gas to CVD reactor 15
And the inflow holes 10 for the carrier gas 14 are positioned to face each other. Also, a dish filled with the organometallic compound 4 as a raw material
16 is the organic metal compound 4 of the raw material filled in
It has such a shape that the surface area does not change even if it is reduced by vaporization. The inflow hole 10 and the outflow hole 12 are formed of the organometallic compound 4 arranged in the vaporization vessel 11.
Are located on the side wall above the dish 16 for filling the powder, and face each other. In addition, the same members as those in FIG. 3 are designated by the same reference numerals.

To explain the method of use, the dish 16 is placed in the vaporization container 11 and sealed, and then the entire vaporization container 11 is submerged in the oil 9 in the oil bath 8. The vaporization container 11 is heated from the oil bath 8 through the oil 9, and is kept at a predetermined vaporization temperature by the thermocouple 5 installed immediately below the vaporization container 11 and the temperature controller 7. A carrier gas 14 whose flow rate is controlled by the mass flow controller 1 is caused to flow into the vaporization vessel 11 through the inflow hole 10 and is introduced into the CVD reaction device 15 through the outflow hole 12 together with the vaporized source gas. In this case, the carrier gas flows in parallel with the surface of the powder of the organometallic compound, so that by supplying the raw material gas to the CVD reactor, it is possible to always maintain a stable supply amount of the raw material gas.

The vaporization container of this embodiment has one carrier gas inflow hole and one carrier gas outflow hole. However, even if a plurality of carrier gas inflow holes and outflow holes are provided, they are the same as long as the gas flow is not disturbed. Needless to say, the effect of can be obtained.

[0023]

As described above, the apparatus for vaporizing and supplying an organometallic compound according to the present invention is such that the surface area of the organometallic compound as a raw material is always constant regardless of the decrease due to the vaporization of the raw material. It is possible to always maintain a stable vaporization amount by filling a shaped dish and flowing the carrier gas in the vaporization vessel containing the dish in parallel with the surface of the powder of the organometallic compound. In addition, when heating the organometallic compound as a raw material, the entire evaporation container is submerged in an oil bath and heated through oil whose temperature changes little, so that the entire evaporation container is extremely stable and has a low evaporation temperature (temperature error is ±
Can be kept within 0.5 ° C). Therefore, there is no change in vaporization amount caused by turbulence of gas flow or temperature gradient,
It is extremely advantageous in practice that a thin film having the same characteristic values can always be obtained under the same conditions.

[Brief description of drawings]

FIG. 1 is a configuration diagram of a vaporization and supply device for an organometallic compound according to an embodiment of the present invention.

FIG. 2 is a configuration diagram of a conventional vaporization and supply device of an organometallic compound.

FIG. 3 is a configuration diagram of another conventional vaporizing and supplying device of an organometallic compound.

[Explanation of symbols]

1 ... masuto controller, 4 ... organometallic compound, 5 ... thermocouple, 7 ... temperature controller, 8 ...
Oil bath, 9 ... Oil, 10 ... Inflow port, 11 ... Vaporization container, 12 ... Outflow port, 13 ... Lid, 14 ... Carrier gas,
15 ... CVD reactor, 16 ... dish.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Eiji Fujii 1006 Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Industrial Co., Ltd.

Claims (4)

[Claims] 1. A vaporization container in a vaporization supply device of a metalorganic compound solid raw material for supplying a CVD raw material gas used in a metalorganic chemical vapor deposition apparatus, and a constant temperature bath for accommodating the vaporization container, comprising: A vaporization supply device for an organometallic compound, characterized in that a vessel for filling powder of the organometallic compound is arranged inside the vessel, and an inlet hole and an outlet hole for a carrier gas are arranged on a side wall of the vaporization vessel. 2. The carrier gas inflow hole and outflow hole
Located on the side wall above the dish filled with the powder of the organometallic compound placed in the vaporization vessel, and by arranging them facing each other, the carrier gas can flow in parallel with the surface of the powder of the organometallic compound. The apparatus for vaporizing and supplying an organometallic compound according to claim 1. 3. The plate filled with the powder of the organometallic compound in the vaporization container has a surface area of the powder of the organometallic compound filled therein which is reduced by vaporization of the powder of the organometallic compound. The apparatus for vaporizing and supplying an organometallic compound according to claim 1, having a shape which is always constant. 4. The vaporization temperature of the powder of the organometallic compound is controlled by heating the vaporization vessel by controlling the temperature of the oil by submerging the entire vaporization vessel in the oil bath as the constant temperature bath. It controls, The vaporization supply apparatus of the organometallic compound of Claim 1 characterized by the above-mentioned.