JP2000226667A - Cvd device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a CVD device suitable for a device for mass-production, preventing the peeling of a Cu film in a gaseous starting material introducing passage part, preventing the generation of particles, easily holding the temp. of gas piping or the like to the uniform one, stably executing the feed of a gaseous starting material to a reaction chamber and maintaining good film forming conditions. SOLUTION: This CVD device employs a liq. raw material 21 of an organic copper complex, and the material is vaporized by a vaporizer 24 and is introduced into a reaction chamber 11 to form a copper film (Cu film) on a substrate 13, and the materials of the inside parts of gas piping 30 and 32 and a valve 26 at a gaseous starting material introducing passage part connecting the space between the vaporizer and the reaction chamber are composed of copper or copper alloys. Copper or copper alloys good in thermal conductivity make better the thermal conductivity of the gas piping themselves, are capable of easily executing uniform temp. holding, improve the stability of the feed of a gaseous starting material to a substrate and prevent the peeling of a Cu film and the generation of particles in the gas piping or the like.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a CVD apparatus for forming a copper film using an organic copper complex as a liquid material,
In particular, the present invention relates to an improvement in a material aspect in relation to a source gas of each member such as a source gas pipe and a valve forming a source gas introduction passage.

[0002]

2. Description of the Related Art In the manufacture of large-scale integrated circuits (LSI), liquid crystal displays (LCD), and the like, there is a process of forming a thin film on the surface of a substrate. In the production of the thin film, a CVD apparatus that forms a film using a chemical reaction of a reactive gas is widely used. According to the CVD apparatus, a source gas is introduced from a source gas supply system to a surface of a substrate placed in a reaction chamber in a heated state, and a thin film is formed on the surface by utilizing a chemical reaction.

In the deposition of a metal material using a CVD method,
In recent years, a method using an organometallic complex that is liquid at normal temperature and normal pressure as a raw material is adopted. Above all, in the field of metal materials for wiring, copper (Cu) having high migration resistance and low specific resistance is regarded as a promising next-generation wiring material.
In a Cu-CVD process for forming a Cu film, as a raw material, for example, copper trimethylvinylsilylhexafluoroacetylacetonate (Cu (hfac) (tmv
An organometallic complex of β-diketone which is liquid at normal temperature and normal pressure as in s)) is used.

[0004]

At present, there is no known Cu-CVD apparatus for performing the above-mentioned Cu-CVD process, which has been established as a mass-production apparatus. Until now, film formation has generally been performed by trial and error using a conventional CVD apparatus. In such a Cu-CVD apparatus, a liquid raw material, Cu (hfac) (tmvs),
While the flow rate is controlled by a liquid flow controller from the storage container, the liquid is supplied to a vaporizer in a liquid state, and is vaporized by the vaporizer, and in a gaseous state, a valve and a gas constituting a source gas introduction flow path portion It is introduced into the reaction chamber through a pipe.
Strictly speaking, the gas piping includes a piping portion connecting between the vaporizer and the valve, and a piping portion connecting between the valve and the reaction chamber.

According to the conventional Cu-CVD apparatus, the conventional apparatus is used as described above, and the gas pipe connecting between the valve for introducing the raw material gas into the reaction chamber and the reaction chamber is provided in the vicinity thereof. It was designed to be exchanged with the parts in short cycles. Therefore, the material of the gas pipe includes
SUS316L (a type of stainless steel) has been used from the viewpoint of ease of processing and assembling, that is, from the viewpoint of assembling easiness that welding to a vacuum component such as another flange can be performed by joining the same kind of metal. However, when manufacturing a Cu-CVD apparatus as an apparatus suitable for mass production, what kind of material is used to form a gas pipe for introducing a source gas as a reactive gas into a reaction chamber is based on a conventional apparatus. Unlike the case where it is used, there is room for careful consideration. Such matters to be considered in terms of material are matters to be examined in the same manner with respect to valves and other gas pipes constituting the raw material gas introduction flow path.

The present applicant has previously filed Japanese Patent Application No. 8-23151.
No. 3 discloses a configuration example of a CVD apparatus (chemical vapor deposition apparatus). As a part of the content disclosed in this patent application, an optimum size of a gas inlet of a gas pipe connecting a vaporizer and a reaction chamber is shown. Furthermore, Japanese Patent Application Laid-Open No. 8-288242 discloses that a portion of a portion exposed to a source gas inside a reaction chamber for performing a CVD process is covered with copper or copper oxide. However, not included in the reaction chamber,
In general, there is no detailed description of the material of the gas pipe for introducing the raw material gas which is considered to be replaced in a short cycle.

On the other hand, a CVD apparatus is used for mass production of Cu-CVD.
When manufactured as an apparatus, the gas pipe for introducing the source gas is not configured as an apparatus member that is exchanged in a short cycle, and the source gas is reacted from the vaporizer for a long time when executing the Cu-CVD process. It is required to function as a gas pipe that continues to be introduced into the chamber. According to this requirement, when the source gas is introduced during film formation, C
Although the u film adheres, it is necessary to prevent the Cu film from peeling off, and in general, a gas pipe is used as a gas pipe for vaporizing a thermally unstable liquid material and achieving stable introduction of the material gas. Must be kept at a uniform and predetermined temperature. The necessity of preventing the peeling of the Cu film and keeping the temperature at a uniform predetermined temperature is required for the entire material gas introduction flow path including the gas pipe.

SUMMARY OF THE INVENTION An object of the present invention is to provide a source gas introduction passage suitable for mass-produced Cu-CVD equipment, to solve the above-mentioned problems, and to provide a source gas introduction passage comprising a gas pipe and a valve. CVD that prevents peeling of the Cu film to prevent generation of particles, easily keeps gas pipes and the like at a uniform temperature, stably supplies source gas to the reaction chamber, and maintains good film forming conditions. It is to provide a device.

[0009]

The CVD apparatus according to the present invention is configured as follows to achieve the above object. This CVD apparatus is an apparatus that uses a liquid organic copper complex as a raw material, vaporizes the organic copper complex in a vaporizer, introduces the organic copper complex into a reaction chamber, and forms a copper film on a substrate. The material of the inner surface portion of the source gas introduction flow path connecting the vaporizer and the reaction chamber, which is in contact with the source gas, is made of copper or copper alloy. The raw material gas introduction flow path portion includes a valve and a raw material gas pipe, and the raw material gas pipe includes a portion between the vaporizer and the valve, and a portion between the valve and the reaction chamber. It is preferable that the source gas pipe included in the source gas introduction passage is made of copper or a copper alloy.
As a result, the material of the inner surface portion becomes copper or a copper alloy. Also, the inner surface of the source gas pipe may be configured to be coated with copper or a copper alloy. Furthermore, the valve itself can be made of copper or copper alloy. It is also preferable that the inner surface portion of the valve, which is in contact with the source gas, is coated with copper or a copper alloy. The valve body, the diaphragm unit, and the diaphragm are the inner surfaces of the valve that come into contact with the source gas. As described above, since copper or a copper alloy having good thermal conductivity was used for the material of the inner surface portion of the raw material gas pipe and the valve which is in contact with at least the raw material gas, the adhesion on the inner surface of the raw material gas pipe and the like is improved, and thus Cu The film is not peeled off, and the thermal conductivity of the raw material gas pipe itself and the valve itself is improved, so that it is possible to easily maintain a desired temperature at a uniform temperature, and to improve the stability of supply of the raw material gas to the substrate. In addition, the replacement cycle of the raw material gas introduction passage can be lengthened, and a highly practical mass production apparatus can be realized.

[0010]

Preferred embodiments of the present invention will be described below with reference to the accompanying drawings.

FIG. 1 schematically shows a configuration of a portion related to the main part of the invention of the CVD apparatus according to the present invention.
This CVD apparatus is a Cu-CVD apparatus, and is an apparatus for depositing a Cu film for wiring on a surface of a substrate disposed in a reaction chamber by a CVD method.

In FIG. 1, reference numeral 11 denotes a reaction chamber, which is formed by a vacuum vessel. A substrate holder 12 is provided at a lower portion inside the reaction chamber 11. The substrate 13 to be processed is disposed on the upper surface of the substrate holder 12 with the surface on which the film is to be formed facing upward. A heating mechanism (not shown) is built in the substrate holder 12, and the substrate 13 on the substrate holder 12 is heated to a required temperature (for example, 200 ° C. or lower).
To hold. An exhaust port 14 is formed on a side wall of the reaction chamber 11, and an exhaust pipe 15 is connected to the exhaust port 14.
6 are connected. The exhaust pipe 15 has an exhaust mechanism 17
Connected to. The inside of the reaction chamber 11 is maintained at a required vacuum state (for example, 10 Torr) by the exhaust mechanism 17. A gas inlet 18 is formed in the ceiling 11 a of the reaction chamber 11 at a position above the substrate holder 12 for introducing a source gas (reactive gas) into the reaction chamber 11. Inside the ceiling 11 a of the reaction chamber 11, an adjustment pipe 19 for introducing the raw material gas into the reaction chamber 11, that is, the front space above the substrate 13 is provided with the gas inlet 18 as a center position. ing. In the adjusting tube 19, a portion connected to the gas inlet 18 is a small-diameter tube body, and is formed such that the diameter gradually increases toward the substrate 13 and has a curved portion. The adjusting pipe 19 is a gas inlet 1
This is a gas flow adjusting tube for causing the source gas introduced from 8 to flow at a predetermined flow in the space in front of the substrate 13. The adjusting tube 19 is a gas introduction device having a shape like a horn of a musical instrument as a whole. The lower end of the adjusting tube 19 is extended to the end of the peripheral portion of the substrate 13, and the end is further folded, for example, and fixed to the ceiling 11 a.

In the case of the present embodiment, the raw material supply mechanism is constituted by one system as an example. Reference numeral 20 denotes a raw material container, in which a liquid raw material 21 of an organocopper complex is stored. In this example, the liquid raw material 21 is, for example, Cu
(Hfac) (tmvs) (copper trimethylvinylsilyl hexafluoroacetylacetonate). He (helium) is provided inside the raw material container 20 by a pipe 22.
Gas is supplied, and a pressure by He gas is applied to the liquid raw material 21. The liquid raw material 21 is pushed out to the liquid pipe 23 by this pressure.

The liquid pipe 23 comprises a raw material container 20 and a vaporizer 24.
Are connected. In this case, the position of the vaporizer 24 is
It is set at a position outside the range in which the canopy (not shown) of the reaction chamber 11 opens and closes. The liquid pipe 23 is a pipe for sending the liquid raw material 21 from the raw material container 20 to the vaporizer 24 in a liquid state. A liquid flow controller 25 is provided in the middle of the liquid pipe 23. From the raw material container 20 to the vaporizer 24
The supply amount of the liquid raw material 21 supplied to is controlled by the liquid flow controller 25. The liquid raw material supplied to the vaporizer 24 is converted into a gaseous phase by the vaporizer 24, and is supplied with a gas pipe 30, a valve 26, and a raw material gas together with a carrier gas such as H ₂ (hydrogen) gas or Ar (argon) gas. Through the gas pipe 32, and further through the gas inlet 18 described above.
Through the adjusting tube 19 to the space in front of the substrate in the reaction chamber 11. As described above, the liquid raw material 21 is introduced into the reaction chamber 11 in the gaseous state through the gas pipe 32 as shown by the arrow 31. In the above configuration, the source gas introduction flow path for introducing the source gas into the reaction chamber 11 is constituted by the valve 26 and the gas pipes 30 and 32.

In the present embodiment, the source gas introducing portion has a single system configuration. However, the shape of the gas pipe 32 is not limited to this, but may be any shape corresponding to the configuration of the source supply mechanism. It is needless to say that it can be manufactured. Gas piping 32
The upper end is connected to the outlet of the valve 26, and the lower end is connected to the gas inlet 18 of the ceiling 11 a of the reaction chamber 11. The above-described gas pipe 32 is made of copper (for example, oxygen-free copper) or a copper alloy as a material. The gas pipe 32 is formed to have a diameter of 1/2 inch or more, more preferably 3/4 inch or more, in order to obtain an appropriate conductance. When assembling the gas pipe 32 for introducing a source gas between the source supply mechanism and the reaction chamber 11, a TIG welding structure is employed.

In the above-mentioned Cu-CVD apparatus, the surface of, for example, one substrate 13 carried into the reaction chamber 11 and mounted on the substrate holder 12 is subjected to CVD using a source gas made based on an organic copper complex. A thin film of Cu (copper) is formed by the method. The substrates 13 are carried into the reaction chamber 11 one by one. As is well known, a load lock chamber (not shown) is connected to a reaction chamber 11 of the CVD apparatus via a gate valve (not shown), and is opened by a substrate transfer arm (not shown). The unprocessed substrate is carried into the reaction chamber 11 from the load lock chamber through the gate valve thus set, and the substrate 13 on which the film forming process has been completed is carried out from the reaction chamber 11 to the load lock chamber.

As described above, in the CVD apparatus according to the present embodiment, since copper or a copper alloy is used for the material of the gas pipe 32, the thermal conductivity of the gas pipe 32 itself is improved as a whole,
As a result, the gas pipe is set to a uniform predetermined temperature (for example, 70 to 8).
(0 ° C.). Further, therefore, the supply of the source gas to the substrate 13 can be stabilized for a long period of time, and good film forming conditions can be maintained for a long period of time, so that an apparatus desirable as a mass production apparatus can be realized.
Further, Cu (copper) adheres to the inner surface of the gas pipe 32 to form a Cu film. However, since the gas pipe 32 itself is made of copper or a copper alloy, the adhesion between the gas pipe 32 and the Cu film is reduced. To prevent the Cu film from peeling off,
Generation of particles that degrade the film quality of the u film can be prevented.

In the above-described embodiment, the entire gas pipe 32 is made of copper or copper alloy. However, only the inner portion of the gas pipe is made of copper or copper alloy, or at least a copper film or copper alloy film is formed on its inner surface. Can also be configured to cover. The coating of the copper film or copper alloy film on the inner surface,
The plating is performed by electrolytic copper plating, for example, with a thickness of 2 to 4 μm. In short, the gas pipe 32 is characterized in that the gas pipe 32 is formed such that the material of at least the inner surface of the gas pipe 32 that is in contact with the source gas is copper or a copper alloy.

The gas pipe 30 is also made of copper or a copper alloy or coated with a copper film or a copper alloy film on its inner surface, similarly to the material characteristics of the gas pipe 32. Thus, the same effect as described above is produced in the gas pipe 30.

The valve 26 also has specific components,
Alternatively, all components of the valve are made of copper or a copper alloy, or the inner surface thereof is coated with a copper film or a copper alloy film. FIG. 2 shows a specific configuration example of the valve 26.
Shown in The valve 26 has a body 4 as a constituent element.
1, a diaphragm 42 and a diaphragm unit 43 are included. In the valve 26, a Cu film is adhered to the inner surface of the gas passage 41a formed in the body 41, the surface of the diaphragm 42, and the surface of the diaphragm unit 43 facing the gas passage 41a. Therefore, in this example, the inner surface of the gas passage 41a formed in the body 41, the surface of the diaphragm 42, the diaphragm unit 4
A copper film or a copper alloy film is coated on an inner surface portion directly in contact with the source gas, such as a surface of a portion facing the gas flow path of No. 3. The inner surface is coated with a copper film or a copper alloy film by electrolytic copper plating, for example, with a thickness of 2 to 4 μm. With this configuration, the above-described effect is produced also for the valve 26.

[0021]

As is apparent from the above description, according to the present invention, the organocopper complex which is a liquid raw material is vaporized, and the obtained raw material gas is reacted in the raw gas introduction flow path portion comprising a gas pipe and a valve. In a CVD apparatus that forms a Cu film on a substrate using a Cu-CVD process by introducing it into a chamber, the material of the inner surface of the gas pipe and the like is made of copper or a copper alloy, so that the gas pipe and the like are uniformly kept at a predetermined temperature. Can be easily performed, whereby the source gas can be stably supplied to the substrate. Therefore, it is possible to form a film for a long time,
A CVD apparatus that mass-produces a u film can be realized. Also, even if a Cu film adheres to the inner surface of a gas pipe or the like due to long-term film formation use, the inner surface portion of the gas pipe or the like is also made of copper or a copper alloy, which is substantially the same material as the Cu film, The peeling of the Cu film can be almost prevented, and the C film deposited on the substrate surface can be prevented.
Generation of particles that degrade the film quality of the u film can be prevented. Thus, the CVD apparatus according to the present invention can be used for a long time without replacing only the gas pipes and the like, eliminating downtime of the apparatus caused by replacing only the gas pipes and the like,
The production efficiency can be increased, and a stable Cu film can be produced with high reproducibility and high yield during the film formation operation, which is ideal for mass production equipment.

[Brief description of the drawings]

FIG. 1 is a configuration diagram showing an embodiment of a CVD apparatus according to the present invention.

FIG. 2 is a longitudinal sectional view showing a specific example of the internal structure of the valve.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 11 Reaction chamber 12 Substrate holder 13 Substrate 18 Gas inlet 19 Regulator tube 20 Material container 21 Liquid material 24 Vaporizer 26 Valve 30, 32 Gas piping

 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Toshiro Kanno 5-8-1, Yotsuya, Fuchu-shi, Tokyo Inside Anelva Co., Ltd. (72) Inventor Nobuyuki Masaki 5-81-1, Yotsuya, Fuchu-shi, Tokyo Anelva Inside the corporation

Claims (6)

[Claims] 1. A CVD apparatus that uses a liquid organic copper complex as a raw material, vaporizes the organic copper complex in a vaporizer, introduces the organic copper complex into a reaction chamber, and forms a copper film on a substrate. A CVD apparatus characterized in that the material of the inner surface portion of the raw material gas introduction flow path connecting the raw material gas and the reaction chamber, which is in contact with the raw material gas, is copper or a copper alloy. 2. The CVD apparatus according to claim 1, wherein the source gas pipe included in the source gas introduction passage is made of copper or a copper alloy. 3. The CVD apparatus according to claim 1, wherein an inner surface of the source gas pipe included in the source gas introduction passage is coated with copper or a copper alloy. 4. The CVD apparatus according to claim 1, wherein a valve included in the raw material gas introduction flow path is made of copper or a copper alloy. 5. The CVD apparatus according to claim 1, wherein an inner surface portion of the valve included in the source gas introduction flow path that is in contact with the source gas is coated with copper or a copper alloy. 6. The CVD apparatus according to claim 5, wherein the inner surface portion of the valve that is in contact with the source gas is a valve body, a diaphragm unit, and a diaphragm.