JP3163347B2 - Vacuum apparatus and thin film forming method using the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vacuum apparatus and a method of forming a thin film using the same, and more particularly, to a method for continuously controlling a gas component or a gas amount or pressure in a reaction chamber even when the pressure in the reaction chamber fluctuates greatly. The present invention relates to a vacuum device that can be estimated, and a thin film forming method capable of controlling the formation speed of a thin film and the ratio of constituent components of the thin film precisely and with good reproducibility using the vacuum device.

[0002]

2. Description of the Related Art In the prior art, a mass spectrometer was directly attached to a reaction chamber provided with an evacuation device to measure gas components and gas amounts, so that the pressure (degree of vacuum) in the reaction chamber greatly changed. In such a case, it was practically impossible to continuously measure gas components and gas amounts in the reaction chamber (for example, see Journal of Crystal Growth 77 (1986) p.
194-199 [North-Holland, Amsterdam]).

[0003]

As described above, the conventional measurement of the gas component or gas amount in the reaction chamber is performed by directly attaching a mass spectrometer to the reaction chamber, which is a vacuum vessel, so that the reaction is measured. If the chamber pressure changes significantly,
The gas component or gas amount in the reaction chamber could not be continuously measured.

An object of the present invention is to solve the above-mentioned problems in the prior art, and to provide a vacuum apparatus capable of continuously estimating a gas component or a gas amount in a reaction chamber even when the pressure in the reaction chamber changes greatly. It is another object of the present invention to provide a thin film forming method capable of controlling the forming speed of the thin film and the ratio of the constituent components of the thin film precisely and with good reproducibility by using the vacuum apparatus.

[0005]

In order to achieve the above object of the present invention, a reaction chamber for measuring a gas component and a gas amount in the reaction chamber is installed in a vacuum vessel connected to a vacuum exhaust device. . The above-mentioned reaction chamber has a substrate support section, a substrate heating section, a raw material introduction section, and a conductance (evacuation resistance).
Provide a variable exhaust hole. The reaction chamber and the vacuum vessel are communicated by an exhaust hole of the reaction chamber. Then, by appropriately adjusting the conductance of the exhaust hole of the reaction chamber, the pressure of a predetermined portion in the vacuum vessel or a predetermined portion of the connection portion between the vacuum vessel and the vacuum exhaust device increases when the raw material is supplied to the reaction chamber. Is always set to 10 to ³ Pa or less. A mass spectrometer or pressure gauge is installed at the above site, and the reaction is determined based on the relationship between the pressure difference between the mass spectrometer or pressure gauge installation part and the reaction chamber, and the analysis data measured by the mass spectrometer or the pressure gauge value. A means for estimating a gas component or a gas amount or a pressure (degree of vacuum) in the room is provided.

According to the present invention, a reaction chamber having at least a substrate support part, a substrate heating part and a raw material introduction part and having an exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber is connected to a vacuum evacuation apparatus. The inside of the vacuum chamber or the vacuum container is evacuated by adjusting the amount of evacuation of the exhaust hole of the reaction chamber by setting the exhaust hole of the reaction chamber to communicate with the inside of the vacuum chamber. At least one near the connection of the device
Pressure is always 1 even when the raw material is supplied to the reaction chamber.
A part where the pressure becomes 0 to ³ Pa or less is formed, a mass spectrometer is installed in the part, and the gas component or gas amount in the reaction chamber is measured by the relation between the pressure difference between the mass spectrometer installation part and the reaction chamber and the mass It is a vacuum apparatus provided with at least means for estimating from analysis data measured by an analyzer. In addition, the present invention provides a vacuum chamber in which a reaction chamber having at least a substrate support section, a substrate heating section, and a raw material introduction section, and having an exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber is connected to a vacuum exhaust device. Installed in a vessel, the exhaust hole of the reaction chamber is configured to communicate with the inside of the vacuum vessel, by adjusting the amount of vacuum exhaust of the exhaust hole of the reaction chamber,
The pressure in at least one part of the vacuum vessel or in the vicinity of the connection between the vacuum vessel and the vacuum evacuation device is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber,
A vacuum apparatus provided with at least means for installing a vacuum gauge in the portion and estimating the pressure in the reaction chamber from the relationship between the pressure difference between the vacuum gauge installation section and the reaction chamber. At least one part of the pressure in the vacuum vessel of the present invention or in the vicinity of the connection part between the vacuum vessel and the vacuum evacuation device is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber. And a vacuum gauge such as an ionization vacuum gauge.

[0007] In the vacuum apparatus of the present invention, it is preferable that the exhaust hole that allows the amount of evacuation of the reaction chamber to be freely adjusted has a structure that allows the size of the cross section of the exhaust hole to be adjusted freely. In addition, by providing a heater for preventing gas adsorption near the connection between the vacuum vessel and the vacuum exhaust device, it is possible to more accurately estimate the gas component, gas amount, or pressure.

Further, the present invention relates to a method for forming various semiconductor thin films and the like using the above-mentioned vacuum apparatus, which supports a predetermined substrate in a reaction chamber and introduces a raw material gas containing a thin film constituent element. Then, in the method of forming a thin film on the substrate, the reaction chamber having an exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber, is installed in a vacuum vessel connected to a vacuum exhaust device, The exhaust hole of the reaction chamber communicates with the inside of the vacuum chamber, and the amount of evacuation of the exhaust hole of the reaction chamber is adjusted to at least one portion in the vacuum vessel or near the connection between the vacuum vessel and the vacuum evacuation device. Pressure is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber, and a mass spectrometer or a pressure gauge is installed in this portion, and the mass spectrometer installation section and the reaction chamber are connected. Relationship between pressure difference and mass spectrometer From the analysis data measured in the above, the gas component, gas amount or pressure in the reaction chamber is estimated, and the gas component, gas amount or pressure is always adjusted to a desired value, and the formation rate of the thin film or the component of the thin film A thin film forming method comprising at least a step of controlling the ratio of the thin film, the formation speed of the thin film, the ratio of the constituent components of the thin film can be controlled precisely and with good reproducibility, and a high-quality semiconductor thin film or the like can be formed. It can be produced.

[0009]

When the degree of vacuum in the vacuum vessel of the vacuum apparatus of the present invention changes greatly, it is not possible to continuously measure the gas components or the gas amount inside the reaction chamber with a mass spectrometer mounted in the vacuum vessel. It is possible. Therefore, a reaction chamber in which a gas component or a gas amount is to be measured is installed in a vacuum vessel connected to a vacuum exhaust device. Since the reaction chamber is provided with a substrate support section, a substrate heating section, a raw material introduction section, and an exhaust hole with variable conductance, the reaction chamber and the vacuum vessel are communicated by the exhaust hole. By appropriately adjusting the conductance of the exhaust hole in the reaction chamber, the pressure is always kept at 10 to ³ even when the raw material is supplied to the reaction chamber, at least in a part of the vacuum vessel or a connection portion between the vacuum vessel and the vacuum exhaust device.
A portion that is equal to or less than Pa is configured. In this way, even when the pressure inside the reaction chamber changes to a high-pressure region where the mass spectrometer cannot be used, the pressure in the region where the mass spectrometer can be used is 10 to ³ Pa or less in the above portion. It will change. Therefore, if a mass spectrometer or pressure gauge is installed in a portion where the pressure is always 10 to ³ Pa or less, the mass spectrometer can be used continuously regardless of the pressure inside the reaction chamber, and the mass spectrometer can be used. It is possible to estimate the gas component or gas amount or pressure (degree of vacuum) in the reaction chamber from the relationship between the pressure in the installation section and the pressure difference between the reaction chamber and the data measured by the mass spectrometer or the pressure value measured by the pressure gauge. It becomes possible.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to the accompanying drawings. <Embodiment 1> FIG. 1 shows an example of the configuration of a vacuum apparatus in this embodiment. This vacuum apparatus is used for crystal growth of a semiconductor, and the pressure in the reaction chamber 1 varies between 10 to ⁸ Pa to 1 Pa depending on the amount of the raw material 12 to be introduced. The conductance (vacuum exhaust resistance) is adjusted appropriately by adjusting the cross-sectional area of the exhaust hole 5 of the reaction chamber 1, and the conductance C between the reaction chamber 1 and the installation location of the mass spectrometer 9 is adjusted.
Is set so that C = 10 to ⁴ m ³ / s. The pumping speed of the vacuum pumping device 3 is 150 l / s = 0.15 m ³ /
s. Further, in order to prevent gas adsorption at the connection portion 4 between the vacuum vessel 2 and the vacuum evacuation device 3, a heater 13 was provided in this portion and heated. Under such conditions, the pressure at the installation location of the mass spectrometer 9 was always 10 to ³ Pa or less. FIG. 3 shows the relationship between the pressure in the reaction chamber 1 and the pressure at the installation position of the mass spectrometer 9 at this time. As shown in the figure, the range in which the mass spectrometer can be used was always obtained, and the gas component or gas amount in the reaction chamber could be estimated from the data of the mass spectrometer. In this embodiment, a semiconductor crystal growth apparatus has been described. However, an etching apparatus or a CVD apparatus in which the pressure in the reaction chamber changes within a range of 10 to ⁸ Pa to 1 Pa.
It is needless to say that the gas component or the gas amount in the reaction chamber can be estimated also in another vacuum apparatus such as an apparatus as in this embodiment.

<Embodiment 2> FIG. 2 shows an example of the configuration of a vacuum apparatus in this embodiment. This vacuum apparatus is used for crystal growth of a semiconductor. The pressure in the reaction chamber 1 is increased from 10 to ⁸ Pa to 1 P depending on the amount of the raw material 12 to be supplied.
a. The conductance is appropriately adjusted by adjusting the cross-sectional area of the exhaust hole 5 of the reaction chamber 1 so that the reaction chamber 1
And the conductance C between the mass spectrometer 16 and the installation location of the mass spectrometer 16 are set so that C = 10 to ⁴ m ³ / s. The evacuation speed of the evacuation device 15 is 150 l / s = 0.1
It was 5 m ³ / s. The connection portion 14 between the vacuum vessel 2 and the vacuum exhaust device 15 was heated by a heater 17 in order to prevent gas adsorption. Under these conditions, the pressure at the installation site of the mass spectrometer is always 1
0 to ³ Pa or less. At this time, the pressure in the reaction chamber 1
FIG. 3 shows the relationship between the mutual pressures at the installation position of the mass spectrometer 16. Therefore, the mass spectrometer 16 can always be used, and the gas component or gas amount in the reaction chamber can be estimated from the data of the mass spectrometer 16.
In the present embodiment, a semiconductor crystal growth apparatus has been described. However, the present embodiment is also applicable to other vacuum apparatuses such as an etching apparatus in which the pressure in a reaction chamber changes in a range of 10 to ⁸ Pa to 1 Pa, or a CVD apparatus. Similarly, it is possible to estimate the gas components or their amounts in the reaction chamber.

<Embodiment 3> This embodiment will be described with reference to the semiconductor crystal growth apparatus shown in FIG. Depending on the amount of the raw material supplied to the reaction chamber 1, the pressure in the reaction chamber 1 is 10
It varies between ⁸ Pa and 1 Pa. The conductance is appropriately adjusted by adjusting the size of the cross section of the exhaust hole 5 of the reaction chamber 1 so that the conductance C between the reaction chamber 1 and the installation location of the ionization gauge 10 is C = 10 to ⁴ m. ³ / s was set. The pumping speed of the vacuum pumping device 3 is 150 l /
s = 0.15 m ³ / s. Heating was performed by the heater 13 in order to prevent gas from adsorbing to the connection portion 4.
Under these conditions, the pressure at the installation location of the ionization gauge 10 was always 10 to ³ Pa or less. Therefore, the ionization gauge 10 can always be used, and the pressure in the reaction chamber 1 can be estimated from the data of the ionization gauge 10.
Assuming that the pressure in the reaction chamber 1 is P ₁ and the pressure at the installation location of the ionization gauge 10 is P ₂ , under these conditions, P ₁ = P ₂
× 1.5 × 10 ³ . In the present embodiment, a semiconductor crystal growth apparatus has been described. However, the present embodiment is also applicable to other vacuum apparatuses such as an etching apparatus in which the pressure in a reaction chamber changes within a range of 10 to ⁸ Pa to 1 Pa, or a CVD apparatus. Similarly, the pressure in the reaction chamber can be estimated.

<Embodiment 4> FIG. 4 shows an example of the configuration of a semiconductor crystal growth apparatus used in this embodiment. The pressure in the reaction chamber 1 varies from 10 to ⁸ Pa to 1 Pa depending on the amount of the raw material for forming a thin film supplied to the reaction chamber 1. The conductance is appropriately adjusted by adjusting the cross-sectional area of the exhaust hole 5 of the reaction chamber 1 so that the conductance C between the reaction chamber 1 and the installation location of the mass spectrometer 9 and the ionization vacuum gauge 10 is C = 1
It was set so as to be 0 to ⁴ m ³ / s. The evacuation speed of the evacuation device 3 was 150 l / s = 0.15 m ³ / s. Heating was performed by the heater 13 in order to prevent gas from adsorbing to the connection portion 4. Under such conditions, the pressure at the installation location of the mass spectrometer 9 and the ionization gauge 10 was always 10 to ³ Pa or less. Therefore, the mass spectrometer 9 and the ionization vacuum gauge 10 could always be used. Then, from the data of the mass spectrometer 9 and the ionization vacuum gauge 10, the gas components and the gas amount in the reaction chamber 1 and the pressure in the reaction chamber 1 could be estimated. Now, assuming that the pressure in the reaction chamber 1 is P ₁ and the pressure at the installation location of the ionization gauge 10 is P ₂ , P ₁ = P ₂ × 1.5 × 10 ³ under the above conditions. . This relationship is shown in FIG.

Using the above-described semiconductor crystal growth apparatus, undoped and Si-doped GaAs
Semiconductor crystals were epitaxially grown. At first,
Non-doped GaAs is grown on a semi-insulating GaAs substrate. First, trimethyl gallium (Ga (CH ₃ ) ₃ ... TMGa) which is a Ga raw material 18 is supplied to the reaction chamber 1 for 5 seconds. During this time, the Ga raw material 18 was adjusted so that the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 was 1 × 10 to ³ Pa.
Adjust the supply of water. Next, the supply of the Ga raw material 18 is stopped, and vacuum evacuation is performed for 5 seconds. Next, arsine (AsH ₃ ) as the As raw material 19 is supplied to the reaction chamber 1 for 5 seconds. During this time, the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 is 1
The supply amount of the As raw material 19 is adjusted so as to be × 10 to ¹ Pa. Next, supply of AsH ₃ is stopped, and the gas is exhausted for 5 seconds. The above operation is defined as one cycle. When the thin film was grown under such conditions, one molecular layer of GaAs could be grown with good reproducibility in one cycle. This is 1
The GaAs 100 molecular layer was grown 00 times.
GaAs doped with Si is grown on the GaAs 100 molecular layer. First, TMGa and Si raw material 2
Monosilane gas (SiH ₄ / H ₂ ; SiH ₄ concentration: 1 ppm) which is 0 is simultaneously supplied to the reaction chamber 1 for 5 seconds. During this time, the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 is 1
× 10 to ³ Pa, the ratio of TMGa to monosilane gas is 10
The supply amount of the raw material is adjusted so as to be 0: 1. Next, the supply of these raw materials is stopped, and exhaust is performed for 5 seconds. Next, As
Arsine (AsH ₃ ) as a raw material is supplied to the reaction chamber 1 for 5 seconds. During this time, the reaction chamber 1 estimated by the ionization vacuum gauge 10 was used.
The supply amount of the raw material is adjusted so that the inside pressure becomes 1 × 10 to ¹ Pa. Next, supply of AsH ₃ is stopped, and the gas is exhausted for 5 seconds. These operations constitute one cycle. When a thin film was grown under such conditions, one molecular layer of GaAs could be grown in one cycle. This is repeated 100 times to obtain a GaAs having an Si concentration of 1 × 10 to ¹⁷ cm ³ .
100 molecular layers could be obtained with good reproducibility. Also, T
By changing the ratio of MGa and monosilane gas, it was possible to dope Si at an arbitrary concentration. In this embodiment, the growth of non-doped and Si-doped GaAs has been described.
Ga, A doped with Si, Se, S, C, Zn, etc.
An epitaxial layer of a semiconductor containing 1, In, As, P, and Sb can be grown in the same manner as in this embodiment. Further, by knowing the gas components in the reaction chamber 1 and the amounts thereof during the growth of the thin film, it was also possible to analyze the reaction process of the source gas.

Example 5 Using a semiconductor crystal growth apparatus shown in FIG. 4, a non-doped and Si-doped AlGaAs (Al composition 25 atomic%) mixed crystal semiconductor was epitaxially grown in the same manner as in Example 4. First, non-doped AlGaAs is grown on a semi-insulating GaAs substrate. Dimethylaluminum hydride (Al (CH ₃ ) ₂ H...
The raw material 18, trimethylgallium (Ga (CH ₃ ) ₃ .
TMGa) and Arsine (As
H ₃ ) is simultaneously supplied to the reaction chamber. During this time, the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 is 1 × 10 to ³ Pa,
DMAlH and TM in reaction chamber 1 measured by mass spectrometer 9
The supply amounts of the respective raw materials were adjusted so that the ratio of Ga became 1: 3. When grown by such a method, Al
GaAs could be grown with good reproducibility at an Al composition of 25%. Also, by changing the ratio between DMAlH and TMGa, AlGaAs having an arbitrary composition can be obtained. This growth was performed for 10 minutes, and AlGaAs was grown to a thickness of 1000 °. On top of this, AlGaAs doped with Si
s (Al composition 25%) is grown. DMAlH and T
MGa, arsine, and a monosilane gas (SiH ₄ / H ₂ ; SiH ₄ concentration: 1 ppm) as the Si raw material 20 are simultaneously supplied to the reaction chamber 1. During this time, the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 is 1 × 10 to ³ Pa, and the mass spectrometer 9
The ratio of DMAlH to TMGa in the reaction chamber 1 in the reaction chamber 1 measured at 1: 3, and the ratio of DMAlH to monosilane gas was 100:
The supply amount of each raw material is adjusted so as to be 1.
A thin film is grown under such conditions, and the Al composition is 25%,
An AlGaAs layer having a Si concentration of 1 × 10 to ¹⁷ cm ³ was obtained with good reproducibility. Also, by changing the ratio between DMAlH and monosilane gas, it was possible to dope Si at an arbitrary concentration. This growth is performed for 10 minutes.
An AlGaAs layer having a thickness of 2,000 mm was grown. In this embodiment, the non-doped and Si-doped AlG
Although the growth of aAs (Al composition: 25%) has been described, Si, Se, S, C, Zn
Ga, Al, In, As, P, Sb doped with
Can be grown in the same manner as in this embodiment. Further, by knowing the gas components in the reaction chamber during the crystal growth and their amounts, the reaction process of the source gas could be analyzed.

Embodiment 6 Using the semiconductor crystal growth apparatus shown in FIG. 4, a non-doped and Si-doped AlGaAs (Al composition 25%) mixed crystal semiconductor was epitaxially grown in the same manner as in Embodiment 4. First, non-doped AlGaAs is grown on a semi-insulating GaAs substrate. First, dimethylaluminum hydride (Al (CH ₃ ) ₂ H... DMAlH) as an Al raw material 21 and trimethyl gallium (Ga (CH ₃ ) ₃ .
MGa) is simultaneously supplied to the reaction chamber 1 for 5 seconds. During this time,
The pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 is 1 × 1
0 ~ ³ Pa, DMA in the reaction chamber 1 as measured by the mass spectrometer 9
The supply amounts of the respective raw materials are adjusted so that the ratio of 1H to TMGa becomes 1: 3. Next, the supply of these raw materials is stopped, and evacuation is performed for 5 seconds. Next, arsine (AsH ₃ ) as the As raw material 19 is supplied to the reaction chamber 1 for 5 seconds. During this time, the supply amount of the raw materials is adjusted so that the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 becomes 1 × 10 to ¹ Pa. Next, supply of AsH ₃ is stopped, and the gas is exhausted for 5 seconds. The above series of operations is defined as one cycle. When such a method is used, AlGaAs (Al composition 2
5%) could be grown with good reproducibility. If the ratio between DMAlH and TMGa is changed, a monolayer of AlGaAs having an arbitrary composition can be obtained. The above cycle was repeated 100 times to grow an AlGaAs 100 molecular layer. Next, SiGaAs-doped AlGaAs (Al composition 25%) was grown on the AlGaAs 100 molecular layer. First, DMAlH and TM
Ga and monosilane gas (SiH ₄
/ H ₂ ; SiH ₄ concentration 1 ppm) is simultaneously supplied to the reaction chamber 1 for 5 seconds. During this time, the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 was 1 × 10 to ³ Pa, and the ratio of DMAlH to TMGa in the reaction chamber 1 measured by the mass spectrometer 9 was 1: 1.
3. The supply amounts of the respective raw materials are adjusted such that the ratio of DMAlH to monosilane gas becomes 100: 1. Next, the supply of these materials is stopped, and the air is exhausted for 5 seconds.
Next, arsine (AsH ₃ ), which is the As raw material 19, was added to 5
Supply to the reaction chamber 1 for seconds. During this time, the supply amount of the raw materials is adjusted so that the pressure in the reaction chamber 1 estimated by the ionization vacuum gauge 10 becomes 1 × 10 to ¹ Pa. Next, supply of AsH ₃ is stopped, and the gas is exhausted for 5 seconds. The above series of operations is defined as one cycle. When the thin film was grown under the above conditions, a monolayer of AlGaAs (Al composition 25%) could be grown with good reproducibility in one cycle. By repeating the above cycle 100 times, the Si concentration is 1 × 10 to
An AlGaAs 100 molecular layer of ¹⁷ cm ~ ³ was obtained with good reproducibility. If the ratio of DMAlH to monosilane gas is changed, Si can be doped at an arbitrary concentration. In this embodiment, the non-doped and Si-doped Al
Although the growth of GaAs (Al composition 25%) has been described,
By changing the raw material, a mixed crystal containing Ga, Al, In, As, P, and Sb doped with Si, Se, S, C, Zn, or the like can be similarly grown. In addition, it was possible to analyze the reaction process of the source gas by knowing the gas components or the gas amount in the reaction chamber during the growth of the thin film.

[0017]

As described in detail above, according to the vacuum apparatus of the present invention, even when the pressure in the reaction chamber changes greatly, the gas component or gas amount in the reaction chamber can be easily changed.
And it can be estimated continuously. Therefore, when forming various thin films using the vacuum apparatus of the present invention,
Since the gas component, gas amount, or pressure in the reaction chamber can be constantly monitored during the formation of the thin film, by controlling these to a desired value, the thin film formation speed or the ratio of the constituent components of the thin film, etc. Can be controlled precisely and with good reproducibility, and a very good quality thin film of a semiconductor or the like can be manufactured.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing the structure of a vacuum device exemplified in Embodiment 1 of the present invention.

FIG. 2 is a schematic diagram showing the structure of a vacuum device exemplified in Embodiment 2 of the present invention.

FIG. 3 is a graph showing a relationship between a pressure in a reaction chamber and a pressure at an installation location of a mass spectrometer as exemplified in the embodiment of the present invention.

FIG. 4 is a schematic view showing a structure of a semiconductor crystal growth apparatus exemplified in Embodiment 4 of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 ... Reaction chamber 2 ... Vacuum container 3 ... Vacuum exhaust device 4 ... Connection part 5 ... Exhaust hole 6 ... Substrate support part 7 ... Substrate heating part 8 ... Raw material Introducing section 9: Mass spectrometer 10: Ionization vacuum gauge 11: Substrate 12: Raw material 13: Heater 14: Connection part 15: Vacuum exhaust device 16: Mass spectrometry Total 17: heater 18: Ga raw material 19: As raw material 20: Si raw material 21: Al raw material

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Kiyoshi Ouchi 1-280 Higashi Koikekubo, Kokubunji-shi, Tokyo Inside the Central Research Laboratory, Hitachi, Ltd. Oki Corporation Sakai Plant (72) Inventor Noriyuki Omori 2-6-40 Chikushinmachi, Sakai-shi, Osaka Daido Oxygen Company Sakai Plant (58) Field surveyed (Int. Cl. ⁷ , DB name) H01L 21 / 205 C30B 23/02 C30B 25/16 H01L 21/203 H01L 21/3065

Claims (6)

(57) [Claims] A vacuum chamber having at least a substrate support section, a substrate heating section and a raw material introduction section, and a reaction chamber having an exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber. It is installed in a vessel, and the exhaust hole of the reaction chamber communicates with the inside of the vacuum vessel, and the amount of evacuation of the exhaust hole of the reaction chamber is adjusted. At least one part of the pressure in the vicinity of the connection part constitutes a part where the pressure is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber. A vacuum apparatus comprising at least means for estimating a gas amount from a relationship between a pressure difference between a mass spectrometer installation section and a reaction chamber and analysis data measured by the mass spectrometer. 2. A vacuum chamber having at least a substrate support section, a substrate heating section, and a raw material introduction section, and a reaction chamber having an exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber. It is installed in a vessel, and the exhaust hole of the reaction chamber communicates with the inside of the vacuum vessel, and the amount of evacuation of the exhaust hole of the reaction chamber is adjusted. At least one part of the vicinity of the connection part constitutes a part where the pressure is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber, and a vacuum gauge is installed in this part to reduce the pressure in the reaction chamber to a vacuum. A vacuum apparatus comprising at least means for estimating from a relationship between a pressure difference between a gauge installation section and a reaction chamber. 3. The vacuum apparatus according to claim 1, wherein a mass spectrometer and a vacuum gauge are provided in a portion where the pressure is always 10 to ³ Pa or less even when the raw material is supplied to the reaction chamber. . 4. The exhaust hole according to claim 1, wherein the exhaust hole capable of freely adjusting the amount of evacuation of the reaction chamber has a mechanism for freely adjusting the size of the opening of the exhaust hole. And vacuum equipment. 5. The vacuum apparatus according to claim 1, wherein a heater for preventing gas adsorption is provided near a connection portion between the vacuum vessel and the vacuum exhaust device. 6. A method of forming a thin film on a substrate by supporting a predetermined substrate in a reaction chamber and introducing a raw material gas containing a thin-film constituent element, wherein the amount of evacuation in the reaction chamber can be adjusted freely. A reaction chamber having an exhaust hole is provided in a vacuum vessel connected to a vacuum exhaust device, and the exhaust hole of the reaction chamber communicates within the vacuum vessel. Is adjusted so that the pressure in at least one portion of the vacuum container or in the vicinity of the connection portion between the vacuum container and the vacuum evacuation device is 10 to ³ P
a portion or less, a mass spectrometer or a pressure gauge is installed in the portion, the relationship between the pressure difference between the mass spectrometer installation section and the reaction chamber, and the analysis data measured by the mass spectrometer, Estimating the gas component, gas amount or pressure in the reaction chamber, adjusting the gas component, gas amount or pressure to always have a desired value, and controlling at least the step of controlling the formation rate of the thin film or the ratio of the constituent components of the thin film. A method of forming a thin film, comprising: