JPH1129870A - Chemical vapor growth device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To solve a problem on safety that a device temp. becoming high and a problem in that vapor of a high temp. reflocculatable raw material cannot be used together with vapor of a low temp. decomposable raw material in a hot wall type chemical vapor growth device. SOLUTION: A conduit tube part equipped with a heating means is extended from a raw material introducing port 17a in a raw material introducing cap 17 through a transport zone 10b into a reaction tube 10 and is equipped with a raw material vapor nozzle 18a in which a discharge port is situated in the vicinity of a growth zone 10a. Vapor of the raw material is transported to the growth zone without being reflocculated in the transport zone, because the conduit tube part is heated to the reflocculation temp. or above of vapor of the raw material, and vapor of the low decomposable raw material is transported to the growth zone while left undecomposed, if supplied from the other raw material introducing port 17b. Thus, a problem, that the external part of the device is heated to the high temp. with a preheater, and a problem, that vapor of a high temp. reflocculatable raw material cannot be used together with vapor of a low temp. decomposable raw material, are solved.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hot wall type chemical vapor deposition (hereinafter, abbreviated as HW-CVD) apparatus, and more particularly to a structure suitable for using a re-agglomerated raw material and a low-temperature decomposable raw material. About.

[0002]

2. Description of the Related Art In a chemical vapor deposition (CVD) method, one or a plurality of source (chemical) vapors generated in a source system are transported to a reactor maintained at a constant pressure, mixed, and heated to a high temperature. This is a method of depositing a thin film by performing a chemical reaction on a held substrate. Since the film formation mechanism is derived from a chemical process, it does not require high temperatures like the thermal oxidation method,
Further, a high vacuum state such as physical vapor deposition (PVD) such as sputtering or resistance wire heating evaporation is not required.
Accordingly, even a large-scale film forming apparatus can be realized at relatively low cost. This film formation method has already been used in a wide range of industries as a means for forming a metal film, a dielectric film, and a semiconductor thin film.

[0003] The CVD apparatus is roughly divided into a reactor system for growing a thin film by heating one or more chemical raw material vapors;
A raw material supply system that generates raw material vapor and supplies the raw material vapor to the reactor via a transport pipe, etc., and an exhaust system that discharges exhaust gas and excess raw material vapor generated in the reactor outside the reactor using a vacuum pump or the like Consists of

FIG. 6 shows an HW-CV widely used at present.
It is sectional drawing which showed the reactor system of D apparatus typically. FIG.
In the figure, 10 indicates that the body part has at least the growth zone 10
This is a large-diameter reaction tube composed of a and a transport zone 10b.
A flange 10c is provided at one end of the large-diameter reaction tube 10 on the side of the transport zone 10b, and has a large opening to allow the susceptor 12 on which the substrate 11 is placed to be taken in and out of the vessel.
The raw material introduction cap 13 is provided in contact with the flange 10a with an O-ring (not shown) sandwiched therebetween. The material introduction cap 13 is connected to the susceptor 12 from the reaction tube 10.
It has a structure that can be removed to make it possible to put in and out. In addition, one or more raw material vapor inlets 13 are provided in the raw material introduction cap 13 in accordance with the number of raw material vapors to be used.
a and 13b (13c for three or more raw materials).
A raw material transport pipe of a raw material supply system is connected to these raw material vapor inlets.

On the other hand, the other end of the reaction tube 10 is greatly constricted to form an exhaust port 10d for exhaust gas and unreacted raw material vapor. The exhaust port is connected to an exhaust system through an exhaust pipe having a relatively large diameter. Reference numeral 14 denotes a cylindrical electric furnace (diffusion furnace) having temperature control means, which is a growth zone 1 of a reaction tube.
0a is provided so as to surround the outer periphery. The cylindrical electric furnace 14 uniformly heats the inside of the growth zone 10a of the reaction tube. On the other hand, the outer periphery of a portion corresponding to the transport zone 10b of the reaction tube is open to the atmosphere, and the cylindrical electric furnace 1
The high heat of 4 prevents the flange 10c and the raw material introduction cap 13 from becoming high in temperature. The transport zone 10b is a heat buffer zone, where no film deposition occurs. Only the raw material vapor is transported.

When the raw material vapor which is coagulable at normal temperature is used, the raw material vapor re-aggregates on the inner wall of the reaction tube in the transport zone 10b to reduce the film deposition rate or to make the film composition unstable. In order to cause a problem, as shown in FIG. 6, a method is widely used in which a cylindrical preheater 15 is provided around the outer periphery of a reaction tube to heat the transport zone 10b to a temperature equal to or higher than the re-agglomeration temperature. For example, see the International Electron Device Meeting (IEEE) Tech
nical Digest, p.684, 1986). The preheater 15 is also provided with a temperature control means, which is controlled at a constant temperature. The set temperature is selected to be equal to or higher than the reagglomeration temperature of the raw material vapor which is most likely to aggregate.

[0007]

SUMMARY OF THE INVENTION Such an HW-CV
The D apparatus is currently widely used for depositing various thin film materials, but the reactor has a plurality of problems as described below, and the solution has been strongly desired. That is, in the conventional example, since the preheater 15 has a structure in which the reactor flange 10c and the raw material introduction cap 14 are heated in a parasitic manner,
The specifications of these thermal designs (the degree of freedom in material selection and structural design) have become strict, which has been a factor that increases the cost of HW-CVD equipment. Further, when the susceptor 12 is taken in and out, an operator may erroneously come into contact with the reactor flange 10c and the raw material introduction cap 14 which have become hot, which is a problem in safety prevention.

Further, in the conventional example, the transport zone 10b of the reactor is uniformly heated in accordance with the temperature of the raw material vapor which is most likely to coagulate in the preheater 15, so that the reactor is decomposed at the set temperature of the preheater 15. Such other raw materials could not be used at the same time. This means that the selection of the CVD raw material is greatly restricted.

The problem will be specifically described by taking an example. For example, dipivaloyl methanate lead Pb (O ₂ C ₁₁ H ₁₉ ) ₂ [which is frequently used to form a PbO (lead oxide) film] Hereinafter, abbreviated as Pb (DPM) ₂ ], the raw material has strong cohesiveness, and the temperature of the preheater 15 needs to be set to about 180 ° C. in order to prevent reaggregation inside the reactor transport zone.
In order to obtain a practical PbO film forming rate by simultaneously supplying O ₂ (oxygen) as a raw material vapor and a general oxidizing agent,
The growth temperature (temperature in the electric furnace) must be raised to 550 ° C. or higher. However, at such a high temperature, PbO undergoes re-evaporation or reduction, and the film becomes an oxygen-deficient film, and desired characteristics cannot be obtained. Conventionally, good Pb with HW-CVD equipment
In order to obtain O, the film formation rate must be reduced, that is, productivity must be sacrificed. If highly reactive O ₃ (ozone) is used in place of O ₂ , high-speed film formation at a lower temperature becomes possible, and a PbO film having both a practical film formation rate and good film quality can be realized. Unfortunately, however, O ₃ easily decomposes above 80 ° C.
Decomposition occurs while passing through the transport zone 10b set at 0 ° C., and becomes O ₂ before reaching the substrate position in the growth zone 10a of the reactor, and the expected effect of O ₃ cannot be obtained. . As described above, in the conventional HW-CVD apparatus, it is impossible to simultaneously use another raw material having a decomposition temperature lower than the re-agglomeration temperature of one raw material used, which is a development of the CVD technology. Was a major stake.

SUMMARY OF THE INVENTION The present invention has been made to solve some or all of the problems relating to the reactor system of the conventional hot wall type CVD apparatus. It is an object of the present invention to provide a reactor which has high operation safety and is suitable for using a re-agglomerated raw material and a low-temperature decomposable raw material.

[0011]

In order to achieve the above object, according to the present invention, a reactor system of an HW-CVD apparatus is configured as described in the claims. That is, in the invention described in claim 1, the conduit portion having the temperature control means extends from the raw material introduction port of the raw material introduction cap into the reaction tube through the transport zone, and the discharge port is located at or near the growth zone. It is configured to have at least one raw material vapor nozzle positioned.

The inventions described in claims 2 to 6 show various configuration examples of the present invention.
Claim 8 shows a configuration example of a raw material steam nozzle having a temperature control means. For example, as shown in an embodiment which will be described later, a heating means capable of controlling the temperature is provided in a conduit portion, and a raw material vapor nozzle having a discharge port at or near a reaction tube growth zone is provided at a raw material introduction port, and a heated raw material is provided. The configuration is such that a raw material vapor having a strong re-coagulation property is injected from a vapor nozzle. In this configuration, since the conduit is heated to a temperature equal to or higher than the re-coagulation temperature of the raw material vapor,
As in the conventional example shown in FIG. 6, not only has the function of transporting the source vapor to the growth zone without causing reaggregation in the reaction tube transport zone, but also only the source vapor nozzle is locally heated. With this configuration, it is possible to solve the problem of the related art in which the reaction tube flange and the raw material introduction cap are heated to a high temperature by the preheater.

In another embodiment, a preheater is provided on the outer periphery of the transport zone, (1) a heating means with a temperature control function is provided in the conduit section when it is not installed, and (2) when the heater is installed, A cooling means having a control function is provided in the conduit portion, and a raw material vapor nozzle having a discharge port at or near the reaction tube growth zone is provided in at least one of the plurality of raw material introduction ports. Is a configuration in which a high-temperature re-coagulable raw material vapor is passed through a raw material vapor nozzle having the heating means, and in the case of the above (2), a low-temperature decomposable raw material vapor is passed through a raw material vapor nozzle having the cooling means. I have. In these configurations, in the case of the above (1), the high-temperature reagglomerated raw material vapor is stably transported to the growth zone through a dedicated raw material vapor nozzle locally heated to a temperature higher than the reagglomeration temperature, The raw material vapor is also stably transported to the growth zone without being heated from the outer periphery of the transport zone. In the case of the above (2), the low-temperature decomposable raw material vapor is stably transported to the growth zone through a dedicated nozzle locally cooled to a temperature lower than the decomposition start temperature. The high-temperature re-coagulable raw material vapor is transported without re-coagulation in the transport zone uniformly heated from the outer periphery by the preheater.

Further, a raw material vapor nozzle having a heating means and a raw material vapor nozzle having a cooling means are used without using a preheater. In the case where the raw material vapor is passed, each raw material vapor is stably transported to the growth zone at an optimum temperature. Therefore, it is possible to use a raw material system containing both a high-temperature re-coagulable raw material vapor and a raw material vapor that decomposes at a temperature lower than the coagulation start temperature of the raw material vapor, and also to improve the safety of work because no preheater is used. I can do it.

As described above, in the configuration of the present invention, the problem of the prior art that the reaction tube flange and the raw material introduction cap are heated to a high temperature by the preheater, and the high temperature reagglomerated raw material and the low temperature decomposable raw material are used. It is possible to solve the problem of the prior art that the raw material systems cannot be used simultaneously.

[0016]

According to the present invention, a thin film can be formed by stably transporting a high-temperature re-coagulable raw material vapor to a reactor growth zone without parasitic heating of a reactor flange or a raw material introduction cap. can do. Further, a thin film can be deposited using a raw material system composed of both a raw material vapor having a high-temperature re-coagulation property and another raw material vapor having a decomposition temperature lower than the re-coagulation temperature of the raw material vapor. Further, an effective film formation can be performed without heating the reactor flange and the material introduction cap, and simultaneously using a high-temperature re-agglomerated material and a low-temperature decomposable material. Therefore, the most suitable raw material for film formation can be selected without being affected by the temperature conditions, and the effect that a high-performance film can be formed at high speed can be obtained. .

[0017]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an HW-CV according to the present invention will be described.
The reactor system of the D apparatus will be described based on an embodiment. Since the present invention is applicable to various types of CVD raw materials and types of films, the configuration is described with generality without specifying the raw materials, and a specific description of the raw materials is given in the description of the effects. I will.

(First Embodiment) FIG. 1 shows a first embodiment of the present invention.
FIG. 4 is a schematic cross-sectional view for describing the embodiment. In FIG. 1, the portions having the same numbers as those in FIG. 6 are the same as those in the conventional example, and have already been described, so that detailed description will be omitted. In FIG. 1, reference numeral 10 denotes a growth zone 10a and a transport zone 10
b, a large-diameter reaction tube having a flange 10c and an exhaust port 10d as constituent elements. Reference numeral 14 denotes a cylindrical electric furnace (diffusion furnace) having temperature control means, which is installed so as to surround the outer periphery of the growth zone 10a of the reaction tube. The outer periphery of the transport zone 10b of the reaction tube is open to the atmosphere. The exhaust port of the reaction tube 10 is a HW-CV by a relatively large exhaust pipe.
It is connected to the exhaust system of device D. The flange 10c has an O
A raw material introduction cap 17 that can be removed by holding a ring (not shown) is attached.

The raw material introduction caps 17 have the same number of raw material vapor introduction ports 17a, 17b, 17c,.
Are connected to a raw material transport pipe (not shown) for transporting the raw material of the raw material supply system to the reactor. From a raw material vapor inlet (17a in FIG. 1 as an example) through which a high-temperature reagglomerated raw material vapor passes, a conduit extends toward the growth zone 10b, and a raw material vapor nozzle 18a provided with heating means is provided around the conduit. I have. Although not shown in FIG. 1, the other material introduction ports 17b, 17c,
In order to introduce the re-coagulable raw material vapor, the raw material vapor nozzles 18b, 18c,... Having the same heating means are provided. This raw material steam nozzle 18a (1
8b, 18c,...) Are temperature-controlled at a temperature slightly higher than the re-coagulation start temperature of the raw material vapor passing through the conduit. The detailed structure of the raw material steam nozzle will be described later.

Hereinafter, the effect of the first embodiment shown in FIG. 1 will be described with reference to the case where PbO is deposited using Pb (DPM) ₂ having high temperature re-aggregation property and O ₃ having low temperature decomposition property as raw material vapor. This will be explained. In this case, Pb (DPM) ₂ vapor is introduced from a raw material inlet 17a provided with a raw material vapor nozzle 18a heated to 180 ° C., and O ₃ is supplied from a raw material vapor inlet (here, 17b) having no raw material vapor nozzle. be introduced. In the present embodiment, Pb (DPM) ₂ moves in the raw material introduction nozzle conduit heated to a temperature higher than the re-agglomeration start temperature 150 ° C., so that Pb (DPM) ₂ does not precipitate in the conduit, and the Pb (DPM) ₂ does not precipitate in the conduit. The growth zone 10a can be reached without being deposited on the wall. That is, the present embodiment has the same function as the conventional example of FIG. 6 in the function of transporting the re-coagulable raw material vapor in the transport zone 10b.

However, as is apparent from the structure shown in FIG. 1, in this embodiment, since the preheater is not provided on the outer peripheral portion of the transport zone 10b, the reaction tube flange 1 is not provided.
0c and the raw material vapor introduction cap 13 are not parasitically heated to a high temperature, and the transport zone 10b is not exposed to a high temperature. That is, the present embodiment solves the problem of the prior art that the thermal design of the material introduction cap is difficult and the worker may come into contact with the heated material introduction cap or the flange. Become.

Further, in the present embodiment, the material vapor nozzle 18
a is heated locally, so that the raw material steam nozzle 18
The low-temperature decomposable vapor passing outside of a can be stably transported from the raw material inlet 17b to the growth zone 10a. That is, in the present embodiment, it is impossible to select a raw material system composed of both a high-temperature re-coagulable raw material vapor and a raw material vapor that decomposes at a temperature lower than the aggregation start temperature of the raw material vapor. This has also been solved.

In this embodiment, the transport zone 10b
The system uses a configuration in which the raw material vapor nozzle is locally heated to prevent re-coagulation of the raw material vapor, so that the power consumption for preventing re-coagulation can be significantly reduced compared to the conventional example in which the entire reaction tube is heated by a pre-heater. It also has advantages.

(Second Embodiment) FIG. 2 is a schematic sectional view for explaining a second embodiment. In FIG. 2, portions having the same numbers as those in FIGS. 6 and 1 are the same as those already described, and detailed description thereof will be omitted. In FIG.
Reference numeral 10 is a large-diameter reaction tube having a growth zone 10a, a transport zone 10b, a flange 10c, and an exhaust port 10d as constituent elements. Reference numeral 14 denotes the above-mentioned cylindrical electric furnace (diffusion furnace) having temperature control means. A preheater 15 is provided on the outer periphery of the reaction tube transport zone 10b. The preheater 15 is controlled so that the inside of the transport zone 10b becomes higher than the aggregation start temperature of the reagglomerated raw material used.
The flange 10c is provided with a raw material introduction cap 19 which can be detached by holding an O-ring (not shown). This raw material introduction cap 19 has raw material vapor introduction ports 19a, 19b, 19c,.
Is opened, and a raw material transport pipe from the raw material supply system is connected.

From a raw material inlet 19b for introducing a raw material vapor which is easily decomposed at a temperature lower than the control temperature of the preheater 15, a conduit extends toward the growth zone 10a, and a raw material vapor nozzle 21b provided with cooling means around the conduit is provided. Is provided. In the case of introducing the low-temperature decomposable raw material vapor to another raw material introduction port, a similar raw material vapor nozzle having a cooling means is provided. These raw material vapor nozzles are controlled to a temperature lower than the decomposition starting temperature of the raw material vapor passing through the conduit. The detailed structure of the raw material steam nozzle will be described later.

The effect of the second embodiment shown in FIG. 2 will be described below by taking as an example the case where PbO is deposited using Pb (DPM) ₂ and low-temperature decomposable O ₃ as raw material vapor. Pb (D
PM) ₂ vapor is introduced from a raw material vapor inlet 19a, and O ₃ is introduced from a raw material inlet 19b having a raw material vapor nozzle 21b whose conduit is cooled to 50 ° C. or lower.

In this embodiment, Pb (DPM) ₂
Passes through the transport zone 10b, which is heated to a temperature higher than the re-agglomeration start temperature 150 ° C. by the preheater 15,
It is possible to reach the growth zone 10a without depositing on the inner wall of the reaction tube. This is the same as the prior art of FIG. However, in the present embodiment, since the low-temperature decomposable O ₃ passes through the inside of the cooled nozzle conduit, it is not exposed to the heat of the preheater 15 in the transport zone 10b, and the growth zone 10a remains as O _3. Can be reached. Therefore, in this embodiment, Pb (D
Both PM) ₂ vapor and O ₃ can be stably transported to the growth zone 10a. As described above, the present embodiment
This solves the problem of the prior art in that it is not possible to select a raw material system composed of a high-temperature re-coagulable raw material vapor and a raw material vapor that decomposes at a temperature lower than the aggregation start temperature of the raw material vapor.

(Third Embodiment) FIG. 3 shows a third embodiment of the present invention.
It is a typical sectional view showing an embodiment. This embodiment has many parts in common with the first embodiment shown in FIG. The parts having the same numbers as those in FIG. 1 are the same and have already been described, so that detailed description is omitted here, and only different parts will be described. The difference between the present embodiment and the first embodiment is that at least one of the raw material introduction ports of the raw material introduction cap 17 (17b in FIG. 3 as an example) has a low-temperature decomposable raw material provided with cooling means around a conduit. Nozzle 22 for steam
b is provided. This cooling means controls the inside of the conduit of the nozzle to be lower than the decomposition temperature of the raw material vapor. The raw material vapor inlet 17a is provided with a nozzle 18a for re-coagulating raw material vapor provided with a heating means around the conduit, and as described above with reference to FIG. The temperature is controlled so that the temperature also becomes higher. The detailed structure of the raw material steam nozzle will be described later.

Hereinafter, the effect of the third embodiment shown in FIG. 3 will be described by taking as an example a case where PbO is deposited using high-temperature reagglomerated Pb (DPM) ₂ and low-temperature decomposable O ₃ as raw material vapor. I do. In this case, Pb (DPM) ₂ vapor is supplied from a raw material inlet 17 a having a raw material vapor nozzle 18 a heated to 180 ° C., and O ₃ is supplied from a raw material vapor nozzle 22 cooled to 50 ° C. or less.
b is introduced from the raw material vapor inlet 17b.

In this embodiment, Pb (DPM) ₂
Moves in the raw material introduction nozzle conduit heated to a temperature higher than the re-coagulation start temperature of 150 ° C., so that it does not precipitate in the conduit and does not precipitate on the inner wall of the reaction tube of the transport zone 10b, and the growth zone 10a can be reached. That is, in the present embodiment, the transporting function of the re-coagulating raw material vapor in the transporting zone 10b has the same function as the conventional example of FIG.

However, in this embodiment, the pre-heater is not provided on the outer peripheral portion of the reaction tube in the transport zone.
As in the conventional example shown in FIG. 1, the reaction tube flange and the raw material vapor introduction cap are not heated to a high temperature parasitically. That is, the present embodiment solves the problems of the prior art that the thermal design of the raw material introduction cap and the reaction tube flange is difficult, and the worker may come into contact with the heated raw material introduction cap and the flange. ing.

Further, in this embodiment, since the low-temperature decomposable O ₃ passes through the inside of the cooled nozzle conduit, the O ₃ is not affected by other parts while passing through the transport zone 10b. ₃ can reach the growth zone 10a. Thus, in the present embodiment, P
Both b (DPM) ₂ vapor and O ₃ can be stably transported to the growth zone 10a. In other words, the present embodiment solves the problem of the prior art in that it is not possible to select a raw material system that simultaneously contains a high-temperature re-coagulable raw material vapor and a raw material vapor that decomposes at a temperature lower than the aggregation start temperature of the raw material vapor. I have.

In the first embodiment shown in FIG. 1, the low-temperature decomposable raw material vapor introduced from the raw material introduction port (eg, 17b) having no raw material vapor nozzle is:
While moving through the transport zone 10b of the reaction tube, the heated raw material vapor nozzle 18a may be touched and decomposed to lower the concentration to some extent. In this regard, in the third embodiment, since the low-temperature decomposable raw material vapor passes through the raw material vapor nozzle 22b having the cooling means, it does not touch the heating nozzle 18a until it reaches the growth zone 10a. There is no possibility of decomposition, and in this respect the first
It is superior to the embodiment of FIG.

As described in the first to third embodiments, the raw material vapor nozzle for passing the raw material vapor having a reagglomeration temperature higher than room temperature (high-temperature reagglomerated raw material vapor) is provided by the above reagglomeration. The raw material vapor nozzle, which is heated to a temperature higher than or equal to the temperature and passes the raw material vapor that decomposes at a temperature lower than the reagglomeration temperature of the high-temperature raw material vapor (low-temperature decomposable raw material vapor), is cooled to a temperature lower than the decomposition temperature. Thus, the respective raw material vapors can be stably transported to the growth zone 10a without precipitation or decomposition.

Next, a specific example of the structure of the raw material vapor nozzle provided with the heating means or the cooling means described in the above embodiments will be described. FIG. 4 is a cross-sectional view of an example of a raw material steam nozzle 18a provided with a heating unit used in the first or third embodiment. In FIG. 4, the material introduction cap 17
The raw material vapor inlet 18a is provided with a raw material vapor nozzle 18a. The raw material vapor nozzle 18a has a structure in which a double pipe of a stainless steel pipe or a quartz pipe sharing a central axis extends straight from the raw material introduction port 17a to the growth zone of the reactor. At the end on the growth zone side, the inner tube 25 of the double tube is open, but the outer tube 26 is welded and sealed at its end to the outer peripheral surface of the inner tube as shown. Therefore, the space surrounded by the outer tube 26 and the inner tube 25 is closed with respect to the inside of the reaction tube.

On the other hand, on the raw material introduction cap side, the inner pipe 25 is connected to a transport pipe (not shown) of the raw material supply system. On the other hand, the outer tube 26 is open to the atmosphere.
In the space between the inner tube 25 and the outer tube 26, a sheath heater 27 wound in a coil shape is installed. Although not shown in the figure, a thin wire sheathed thermocouple for detecting the temperature of the inner tube is also accommodated in a region between the inner tube 25 and the outer tube 26. By externally supplying power to the sheath heater 27 while monitoring the temperature of the inner tube with this thermocouple and generating heat, the inside of the inner tube can be heated to a predetermined temperature. The raw material vapor sent from the raw material supply system is stably transported through the heated inner tube 25 to the growth zone of the reaction tube.

Next, FIG. 5 is a sectional view of another example of the raw material steam nozzle provided with the temperature control means used in the first to third embodiments. This raw material steam nozzle can be heated or cooled (for example, 18a, 2
1b and 22b). This raw material vapor nozzle has a structure in which a triple tube of a stainless steel tube or a quartz tube sharing a central axis extends straight from the raw material introduction port to the growth zone of the reactor.

If the innermost tube of the triple tube is called an inner tube 28, the outermost tube is called an outer tube 29, and the middle tube is called a middle tube 30, the inner tube 28 is located at the end on the growth zone side. However, the outer tube 26 is welded and sealed at its end to the outer peripheral surface of the inner tube, and the space surrounded by the outer tube and the inner tube is isolated from the inside of the reaction tube. The end of the middle tube 30 on the growth zone side is open to a space surrounded by the outer tube 29 and the inner tube 28.

On the other hand, at the end on the raw material vapor introduction cap 17 side, the inner pipe 28 is connected to a transport pipe (not shown) of the raw material supply system. Arrows indicate the flow of temperature-regulated fluid (fluid adjusted to a predetermined temperature by the temperature control means: liquid or gas). For example, when the control temperature is 50 ° C. or higher, a fluid that can withstand high temperatures, such as silicone oil, water is used in a temperature range from room temperature to about 50 ° C., and in a temperature range lower than room temperature, An antifreeze containing ethylene glycol or the like can be used.

Reference numeral 31 denotes a temperature control fluid inlet provided in a space surrounded by the inner pipe 28 and the middle pipe 30, and 32 denotes a middle pipe 30.
And a temperature control fluid outlet provided in a space partitioned by the outer pipe 29 and the outer pipe 29. Outside the reactor, there is provided a constant temperature bath (not shown) having a function of heating or cooling the temperature-regulated fluid to a predetermined temperature and sending it at a predetermined flow rate. A fluid return port is provided. The fluid outlet is connected to a temperature control fluid inlet 31 of the raw material vapor nozzle, and the fluid return port is connected to a temperature control fluid outlet 32 of the raw material vapor nozzle by a flow pipe covered with a heat insulating material.

The high-temperature reagglomerated or low-temperature decomposable raw material vapor sent from the raw material supply system is transported to the growth zone of the reaction tube through the inner tube 28 during the film formation. At this time, the temperature-regulated fluid from the constant temperature bath maintained at a predetermined temperature is sent out from the fluid delivery port, guided to the fluid injection port 31 of the raw material vapor nozzle, and surrounded by the inner pipe 28 and the middle pipe 30. Flows toward the growth zone, turns back at the end of the raw material vapor nozzle, and then flows through a space surrounded by the middle pipe 30 and the outer pipe 29, and exits from the temperature control fluid discharge port 32 of the raw material vapor nozzle. Return to the thermostatic bath through the reflux port. Since the inside of the inner tube 28 is surrounded by the temperature control fluid constantly sent from the constant temperature bath, the temperature of the temperature control fluid is substantially maintained. If a raw material vapor nozzle having such a temperature control means is used, even if the raw material vapor has a high-temperature re-aggregation property or a low-temperature decomposability, it does not re-aggregate or decompose, and the transport zone of the reactor can be stabilized. Can be transported.

[Brief description of the drawings]

FIG. 1 is a schematic cross-sectional view showing a first embodiment of a chemical vapor deposition apparatus according to the present invention.

FIG. 2 is a schematic sectional view showing a second embodiment of the chemical vapor deposition apparatus according to the present invention.

FIG. 3 is a schematic sectional view showing a third embodiment of the chemical vapor deposition apparatus according to the present invention.

FIG. 4 is a schematic sectional view showing one embodiment of a raw material steam nozzle having a heating means according to the present invention.

FIG. 5 is a schematic sectional view showing another embodiment of a raw material vapor nozzle having a temperature control means according to the present invention.

FIG. 6 is a schematic sectional view of an example of a conventional chemical vapor deposition apparatus.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 10 ... Reaction tube 10a ... Reaction tube growth zone 10b ... Reaction tube transportation zone 10c ... Reaction tube flange 10b ... Reaction tube exhaust port 11 ... Substrate 12 ... Susceptor 13 ... Material introduction cap 13a, 13b, 13c ... Material introduction Mouth 14 ... Electric furnace 15 ... Preheater 17 ... Material introduction cap 17a, 17b, 17c ... Material introduction port 18a ... Material vapor nozzle provided with temperature control means (heating control) 19 ... Material introduction cap 20a, 20b, 20c ... Material introduction Ports 21b, 22b: Raw material steam nozzle with temperature control means 25 ... Inner tube of raw material steam nozzle with heating means 26 ... Outer pipe of raw material steam nozzle with heating means 27 ... Seed heater 28 ... Raw material with temperature control means Inner tube of steam nozzle 29 ... Outer tube of raw material steam nozzle having temperature control means 30 ... Has temperature control means Medium pipe of raw material steam nozzle 31 ... Temperature control fluid inlet 32 ... Temperature control fluid outlet

Claims (8)

[Claims] 1. A flat material introduction cap having at least one material vapor introduction port, a flange portion having one end in close contact with the material introduction cap, a body portion, and a tail tube portion serving as a discharge port at the other end. And
A reaction tube comprising at least a transport zone and a growth zone in the order in which the body portion is closer to the flange portion; and a heating device provided to surround the periphery of the growth zone in order to uniformly heat the inside of the growth zone of the reaction tube. A hot-wall type chemical vapor deposition apparatus comprising: a conduit portion having a temperature control means extending from the material introduction port of the material introduction cap through the transport zone into the reaction tube, and A chemical vapor deposition apparatus comprising at least one source vapor nozzle having a discharge port located at or near said growth zone. 2. A temperature of a raw material vapor nozzle having said temperature control means is set to a temperature higher than a reagglomeration temperature of raw material vapor passing through said nozzle.
3. The chemical vapor deposition apparatus according to claim 1. 3. The chemical vapor according to claim 1, wherein the temperature of the raw material vapor nozzle having the temperature control means is set to a temperature lower than the decomposition temperature of the raw material vapor passing through the nozzle. Phase growth equipment. 4. A raw material vapor having a reagglomeration temperature higher than room temperature is supplied to a raw material inlet provided with a raw material vapor nozzle according to claim 2, and the raw material vapor is supplied at a temperature lower than the raw material vapor reagglomeration temperature. The chemical vapor phase according to any one of claims 1 to 3, wherein another raw material vapor to be decomposed is supplied to another raw material inlet which is not provided with the raw material vapor nozzle according to claim 2. Growth equipment. 5. A chemical vapor deposition apparatus which is provided so as to surround a position of a transport zone in said reaction tube from an outer periphery thereof and which is provided with a preheater for heating said reaction tube, and re-aggregates to a higher temperature side than room temperature. The raw material vapor nozzle according to claim 3, wherein the raw material vapor having a temperature is supplied to a raw material introduction port having no raw material vapor nozzle, and another raw material vapor having a decomposition temperature lower than a reagglomeration temperature of the raw material vapor is provided. 4. The method according to claim 1, wherein the raw material is supplied to another raw material introduction port provided with:
The chemical vapor deposition apparatus according to any one of the above. 6. A raw material inlet having a raw material vapor nozzle according to claim 2, wherein at least one raw material vapor having a reagglomeration temperature higher than room temperature is supplied to said raw material vapor inlet. The other raw material vapor decomposed at a low temperature is supplied to another raw material inlet provided with the raw material vapor nozzle according to claim 3. Chemical vapor deposition equipment. 7. The raw material steam nozzle according to claim 2, having a double pipe structure comprising an inner pipe and an outer pipe sharing a central axis,
The material vapor is passed through the inner tube, a region surrounded by the inner tube and the outer tube is cut off from the inside of the reaction tube, and the region is provided with a temperature measuring means and a sheathed heater wound in a coil shape. Characteristic chemical vapor deposition equipment. 8. The raw material steam nozzle according to claim 2 or 3, having a triple pipe structure composed of an inner pipe, a middle pipe, and an outer pipe sharing a central axis, and passing the raw material vapor through the inner pipe. The region surrounded by the inner tube and the middle tube and the region surrounded by the middle tube and the outer tube is cut off from the inside of the reaction tube, and is a raw material vapor nozzle having a function of refluxing a constant temperature fluid from the outside to the region. Chemical vapor deposition apparatus.