CN112281140A - Atomic layer deposition system with double chambers and process - Google Patents
Atomic layer deposition system with double chambers and process Download PDFInfo
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- CN112281140A CN112281140A CN201910677561.8A CN201910677561A CN112281140A CN 112281140 A CN112281140 A CN 112281140A CN 201910677561 A CN201910677561 A CN 201910677561A CN 112281140 A CN112281140 A CN 112281140A
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- outer chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45561—Gas plumbing upstream of the reaction chamber
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to an atomic layer deposition system with double chambers and a process thereof, comprising an outer chamber, wherein the top of the outer chamber is provided with an upper cover which can be opened and closed, the side wall of the outer chamber is provided with an outer chamber air inlet pipe and an outer chamber exhaust pipe, the middle part in the outer chamber is provided with an inner chamber which is taken from the upper cover and provided with an inner chamber air inlet pipe and an inner chamber exhaust pipe; the inner sides of the upper cover and the side wall of the outer chamber are respectively provided with an upper cover heater and a side wall heater, and the inner part of the outer chamber, which is positioned at the bottom of the inner chamber, is provided with a central heater. The invention reduces the oxygen content of the system, is convenient for maintaining and replacing the deposition chamber and improves the application range of the equipment.
Description
Technical Field
The invention relates to the technical field of vacuum film preparation equipment, in particular to an atomic layer deposition system with double chambers and a process.
Background
An atomic layer deposition technique, which is one of thin film deposition techniques, is a method of preparing a target thin film on a sample surface by alternately introducing an organometallic compound and an oxidizing agent into a vacuum chamber under vacuum, isolating the atmosphere of the organometallic compound and the oxidizing agent with a carrier gas, and performing a self-limiting surface reaction of the organometallic compound and the oxidizing agent. In the process, the film growth can be generated on all the surfaces of the organic metal compound and the oxidant precursor which are in mixed contact, so that extremely high requirements are provided for the maintenance of a cavity, and the conventional single-cavity atomic layer deposition equipment needs frequent cavity disassembly for maintenance so as to ensure that the inner wall of the cavity is not stripped; meanwhile, atomic layer deposition is used as a low vacuum coating technology, and the problems of over-high oxygen content and the like exist in the growth of non-oxides such as nitrides, simple substances and the like.
Disclosure of Invention
The applicant aims at the defects in the prior art and provides an atomic layer deposition system and an atomic layer deposition process with double chambers, which are reasonable in structure, so that the oxygen content of a reaction chamber is reduced, and the reaction chamber is convenient to disassemble, replace and maintain.
The technical scheme adopted by the invention is as follows:
an atomic layer deposition system with double chambers comprises an outer chamber, wherein the top of the outer chamber is provided with an upper cover which can be opened and closed, the side wall of the outer chamber is provided with an outer chamber air inlet pipe and an outer chamber exhaust pipe, the middle part in the outer chamber is provided with an inner chamber which is taken from the upper cover, and the inner chamber air inlet pipe and the inner chamber exhaust pipe are arranged on the inner chamber; the inner sides of the upper cover and the side wall of the outer chamber are respectively provided with an upper cover heater and a side wall heater, and the inner part of the outer chamber, which is positioned at the bottom of the inner chamber, is provided with a central heater.
As a further improvement of the above technical solution:
the input end of the inner chamber air inlet pipe is connected with a precursor injection pipe and a carrier gas inlet pipe in parallel.
The precursor injection pipe is provided with at least two groups of precursor modules for containing precursor substances.
The structure of inner chamber does: the device comprises a top cover and a bottom groove which is matched with the top cover to form a closed cavity, wherein a sample groove is arranged in the bottom groove, and an air inlet interface and an air exhaust interface which are respectively communicated with an inner cavity air inlet pipe and an inner cavity exhaust pipe are arranged on two sides of the edge of the bottom groove.
The outer chamber exhaust tube and the inner chamber exhaust tube are both connected with a vacuumizing device.
The outer chamber gas inlet pipe, the precursor injection pipe and the carrier gas inlet pipe are all provided with a flowmeter and a valve.
The outer chamber and the inner chamber are both provided with vacuum gauges.
The upper cover heater, the side wall heater and the central heater are all heated by an armored heating plate and a reflecting plate heating wire or an infrared heater.
The process of the atomic layer deposition system with the double chambers specifically comprises the following steps:
the method comprises the following steps: respectively inflating the outer chamber and the inner chamber to standard atmospheric pressure through an outer chamber air inlet pipe and a carrier gas inlet pipe, opening an upper cover of the outer chamber, taking out the inner chamber, opening a top cover and placing a sample in a sample groove;
step two: the inner chamber is closed and then is placed back into the outer chamber, the upper cover is closed, and the outer chamber and the inner chamber are vacuumized simultaneously by starting the vacuumizing device;
step three: opening an upper cover heater, a side wall heater and a central heater to preheat the inner chamber, and heating the sample to the temperature required by the deposition target;
step four: introducing carrier gas into the inner cavity through the carrier gas inlet pipe, so that the process pressure required by atomic layer deposition is achieved in the inner cavity and the outer cavity; introducing carrier gas into the outer chamber through the air inlet pipe of the outer chamber, so that the pressure in the outer chamber is greater than or equal to the pressure in the inner chamber;
step five: opening a precursor module on the precursor injection pipe, alternately introducing a precursor A and a precursor B, and finishing film deposition on the surface of the sample;
step six: turning off the carrier gas and the heater to cool the system;
step seven: after the temperature is reduced to the room temperature, the outer chamber and the inner chamber are respectively inflated to the standard atmospheric pressure through an outer chamber air inlet pipe and a carrier gas inlet pipe, an upper cover of the outer chamber is opened, and the inner chamber is taken out;
step eight: opening the inner chamber and taking out a sample;
step nine: closing the inner chamber, replacing the outer chamber and closing the outer chamber;
step ten: and (5) extracting vacuum of the inner chamber and the outer chamber, and finishing deposition.
In the second step, the outer chamber and the inner chamber are vacuumized until the pressure ranges from 10 < -3 > Torr to 10 Torr; in the third step, the temperature range of the preheating inner chamber is 20-1000 ℃; the carrier gas adopts O2、N2、Ar2、H2Nitrogen-hydrogen mixed gas or argon-hydrogen mixed gas.
The invention has the following beneficial effects:
the invention has compact and reasonable structure, convenient operation, double-chamber structure of the inner chamber and the outer chamber, independent gas circulation system, and isolation of the closed space from the external environment, thereby greatly reducing the oxygen content. The inner chamber can be disassembled, so that the maintenance of a deposition chamber (sample groove) in the inner chamber is facilitated, the practicability is enhanced, a new scheme is provided for a process for preparing a high-quality thin film, and meanwhile, the device can be used for multiple purposes such as catalytic material preparation, semiconductor material preparation, solar photovoltaic device preparation and the like, and is wide in application range.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural view of the inner chamber of the present invention.
Wherein: 1. an outer chamber air inlet pipe; 2. an upper cover; 3. an outer chamber; 4. an upper cover heater; 5. a sidewall heater; 6. an inner chamber; 7. an inner chamber exhaust tube; 9. an outer chamber exhaust tube; 10. an inner chamber air inlet pipe; 11. a central heater; 12. a vacuum pumping device; 101. a precursor injection pipe; 102. a carrier gas inlet pipe; 61. a top cover; 62. a sample tank; 63. an air inlet interface; 64. an air exhaust interface.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
As shown in fig. 1, the atomic layer deposition system with two chambers according to this embodiment includes an outer chamber 3, an upper cover 2 capable of being opened and closed is disposed at the top of the outer chamber 3, an outer chamber air inlet pipe 1 and an outer chamber air exhaust pipe 9 are disposed on the sidewall of the outer chamber 3, an inner chamber 6 taken from and placed on the upper cover 2 is disposed in the middle of the outer chamber 3, and an inner chamber air inlet pipe 10 and an inner chamber air exhaust pipe 7 are disposed thereon; an upper cover heater 4 and a side wall heater 5 are respectively arranged on the inner sides of the upper cover 2 and the side wall of the outer chamber 3, and a central heater 11 is arranged at the bottom of the inner chamber 6 in the outer chamber 3.
The input end of the inner chamber gas inlet pipe 10 is connected in parallel with a precursor injection pipe 101 and a carrier gas inlet pipe 102.
At least two groups of precursor modules for containing precursor substances are arranged on the precursor injection pipe 101.
As shown in fig. 2, the inner chamber 6 has a structure of: the device comprises a top cover 61 and a bottom groove which is matched with the top cover 61 to form a closed cavity, wherein a sample groove 62 is arranged in the bottom groove, and an air inlet interface 63 and an air outlet interface 64 which are respectively communicated with an inner cavity air inlet pipe 10 and an inner cavity exhaust pipe 7 are arranged on two sides of the edge of the bottom groove.
The outer chamber exhaust tube 9 and the inner chamber exhaust tube 7 are both connected with a vacuum pumping device 12.
The outer chamber gas inlet pipe 1, the precursor injection pipe 101 and the carrier gas inlet pipe 102 are all provided with a flowmeter and a valve.
The outer chamber 3 and the inner chamber 6 are both internally provided with vacuum gauges.
The upper cover heater 4, the side wall heater 5 and the central heater 11 are all heated by an armored heating plate and a reflecting plate heating wire or an infrared heater.
An inert gas circulating system is formed in an outer chamber 3 through an outer chamber air inlet pipe 1 and a chamber exhaust pipe 9, and an upper cover is rotatably connected to a body of the outer chamber 3 and is sealed mechanically; the top cover 61 and the bottom groove of the inner cavity 6 are mechanically sealed, a plurality of groups of precursor modules can be arranged according to actual conditions, and the vacuumizing device 12 can adopt equipment such as a molecular pump set, a dry vacuum pump, a Roots pump set, a condensation pump set and the like.
The specific embodiment of the process of the atomic layer deposition system with the double chambers is as follows:
the first embodiment is as follows:
1) respectively loading trimethylaluminum and deionized water in the precursor module, respectively inflating the inner chamber 6 and the outer chamber 3to a standard atmospheric pressure, opening the upper cover 2, taking out the inner chamber 3 and placing a sample in the sample tank 62;
2) the inner chamber 6 is closed and put back into the outer chamber 3, the upper cover 2 is closed, the vacuum extractor 12 is opened to simultaneously extract the inner chamber 6 and the outer chamber 3 until the vacuum is 5.10-3torr；
3) Preheating the inner chamber 6 by the upper cover heater 4, the side wall heater 5 and the central heater 11, and heating the sample to 200 ℃;
4) introducing high-purity nitrogen into the inner chamber 6 through a carrier gas inlet pipe 102 to enable the pressure in the inner chamber 6 to reach 0.2torr, and introducing carrier gas into the outer chamber 3 through an outer chamber gas inlet pipe 1to enable the pressure in the outer chamber 3to be more than or equal to the pressure in the inner chamber 6;
5) starting a precursor module, alternately introducing a precursor trimethylaluminum and deionized water, and finishing the deposition of an aluminum oxide film on the surface of a sample;
6) closing the high-purity nitrogen gas and the upper cover heater 4, the side wall heater 5 and the central heater 11 to cool the system;
7) after the temperature is reduced to the room temperature, the inner chamber 6 and the outer chamber 3 are respectively inflated to the standard atmospheric pressure, the upper cover 2 is opened, and the inner chamber 6 is taken out;
8) the top cover 61 is opened, and the sample is taken out;
9) closing the inner chamber 6, replacing it in the outer chamber 3, closing the upper lid 2;
10) vacuum is simultaneously drawn on the inner chamber 6 and the outer chamber 3, and deposition is finished.
Example two:
1) loading tetra-diamine hafnium methyl (heated to 75 ℃) and deionized water in the precursor module respectively, inflating the inner chamber 6 and the outer chamber 3to standard atmospheric pressure respectively, opening the upper cover 2, taking out the inner chamber 3 and placing a sample in the sample tank 62;
2) the inner chamber 6 is closed and put back into the outer chamber 3, the upper cover 2 is closed, the vacuum extractor 12 is opened to simultaneously extract the inner chamber 6 and the outer chamber 3 until the vacuum is 5.10-3torr；
3) Preheating the inner chamber 6 by the upper cover heater 4, the side wall heater 5 and the central heater 11, and heating the sample to 100 ℃;
4) introducing high-purity nitrogen into the inner chamber 6 through a carrier gas inlet pipe 102 to enable the pressure in the inner chamber 6 to reach 0.1torr, and introducing carrier gas into the outer chamber 3 through an outer chamber gas inlet pipe 1to enable the pressure in the outer chamber 3to be more than or equal to the pressure in the inner chamber 6;
5) starting a precursor module, alternately introducing a precursor tetra-diamine methyl hafnium and deionized water, and finishing the deposition of a hafnium oxide film on the surface of the sample;
6) turning off the high-purity nitrogen and each heater, and cooling the system;
7) after the temperature is reduced to the room temperature, the inner chamber 6 and the outer chamber 3 are respectively inflated to the standard atmospheric pressure, the upper cover 2 is opened, and the inner chamber 6 is taken out;
8) the top cover 61 is opened, and the sample is taken out;
9) closing the inner chamber 6, replacing it in the outer chamber 3, closing the upper lid 2;
10) vacuum is simultaneously drawn on the inner chamber 6 and the outer chamber 3, and deposition is finished.
The above description is intended to be illustrative and not restrictive, and the scope of the invention is defined by the appended claims, which may be modified in any manner within the scope of the invention.
Claims (10)
1. An atomic layer deposition system having a dual chamber, comprising: the device comprises an outer chamber (3), wherein the top of the outer chamber is provided with an upper cover (2) which can be opened and closed, the side wall of the outer chamber (3) is provided with an outer chamber air inlet pipe (1) and an outer chamber air exhaust pipe (9), the middle part in the outer chamber (3) is provided with an inner chamber (6) taken from the upper cover (2), and the inner chamber air inlet pipe (10) and the inner chamber air exhaust pipe (7) are arranged on the inner chamber;
the inner sides of the upper cover (2) and the side wall of the outer chamber (3) are respectively provided with an upper cover heater (4) and a side wall heater (5), and the inner part of the outer chamber (3) is positioned at the bottom of the inner chamber (6) and is provided with a central heater (11).
2. The atomic layer deposition system with dual chambers of claim 1, wherein: the input end of the inner chamber gas inlet pipe (10) is connected with a precursor injection pipe (101) and a carrier gas inlet pipe (102) in parallel.
3. The atomic layer deposition system with dual chambers of claim 2, wherein: at least two groups of precursor modules for containing precursor substances are arranged on the precursor injection pipe (101).
4. The atomic layer deposition system with dual chambers of claim 2, wherein: the structure of the inner chamber (6) is as follows: the device comprises a top cover (61) and a bottom groove which is matched with the top cover (61) to form a sealed cavity, wherein a sample groove (62) is arranged in the bottom groove, and an air inlet interface (63) and an air exhaust interface (64) which are respectively communicated with an inner cavity air inlet pipe (10) and an inner cavity exhaust pipe (7) are arranged on two sides of the edge of the bottom groove.
5. The atomic layer deposition system with dual chambers of claim 2, wherein: the outer chamber exhaust tube (9) and the inner chamber exhaust tube (7) are both connected with a vacuum pumping device (12).
6. The atomic layer deposition system with dual chambers of claim 2, wherein: and the outer chamber gas inlet pipe (1), the precursor injection pipe (101) and the carrier gas inlet pipe (102) are respectively provided with a flowmeter and a valve.
7. The atomic layer deposition system with dual chambers of claim 1, wherein: the outer chamber (3) and the inner chamber (6) are internally provided with vacuum gauges.
8. The atomic layer deposition system with dual chambers of claim 1, wherein: the upper cover heater (4), the side wall heater (5) and the central heater (11) are all heated by an armored heating plate and a reflecting plate heating wire or infrared heaters.
9. A process for utilizing an atomic layer deposition system having two chambers according to claim 1, wherein: the method specifically comprises the following steps:
the method comprises the following steps: respectively inflating the outer chamber (3) and the inner chamber (6) to standard atmospheric pressure through an outer chamber air inlet pipe (1) and a carrier gas inlet pipe (102), opening an upper cover (2) of the outer chamber (3), taking out the inner chamber (6), opening a top cover (61) and placing a sample in a sample groove (62);
step two, the inner chamber (6) is closed and then placed back into the outer chamber (3), the upper cover (2) is closed, and the outer chamber (3) and the inner chamber (6) are vacuumized simultaneously by starting the vacuumizing device (12);
step three: starting an upper cover heater (4), a side wall heater (5) and a central heater (11), preheating an inner chamber (6), and heating a sample to a temperature required by a deposition target;
step four: introducing carrier gas into the inner chamber (6) through a carrier gas inlet pipe (102) to enable the inner chamber (6) and the outer chamber (6) to reach the process pressure required by atomic layer deposition, introducing the carrier gas into the outer chamber (3) through an outer chamber gas inlet pipe (1), and enabling the pressure in the outer chamber (3) to be more than or equal to the pressure in the inner chamber (6);
step five: opening a precursor module on a precursor injection pipe (101), alternately introducing a precursor A and a precursor B, and finishing film deposition on the surface of the sample;
step six: closing the carrier gas, closing the upper cover heater (4), the side wall heater (5) and the central heater (11) to cool the system;
step seven: after the temperature is reduced to the room temperature, the outer chamber (3) and the inner chamber (6) are respectively inflated to the standard atmospheric pressure through the outer chamber air inlet pipe (1) and the carrier gas inlet pipe (102), the upper cover (2) of the outer chamber (3) is opened, and the inner chamber (6) is taken out;
step eight: opening the inner chamber (6) and taking out the sample;
step nine: closing the inner chamber (6), replacing the outer chamber (3) and closing the outer chamber (3);
step ten: and (5) extracting the vacuum of the inner chamber (6) and the outer chamber (3) and finishing the deposition.
10. The atomic layer deposition process having a dual chamber of claim 9, wherein: in the second step, the outer chamber (3) and the inner chamber (6) are vacuumized to reach the pressure range of 10-3Torr to 10 Torr; in the third step, the temperature range of the preheating inner chamber (6) is 20-1000 ℃; the carrier gas adopts O2、N2、Ar2、H2Nitrogen-hydrogen mixed gas or argon-hydrogen mixed gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910677561.8A CN112281140B (en) | 2019-07-25 | 2019-07-25 | Atomic layer deposition system with double chambers and process |
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| CN201910677561.8A CN112281140B (en) | 2019-07-25 | 2019-07-25 | Atomic layer deposition system with double chambers and process |
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| CN112281140A true CN112281140A (en) | 2021-01-29 |
| CN112281140B CN112281140B (en) | 2022-09-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116791064A (en) * | 2023-06-27 | 2023-09-22 | 江苏迈纳德微纳技术有限公司 | Atomic layer deposition method for laminated perovskite solar cell |
| CN117878043A (en) * | 2024-03-11 | 2024-04-12 | 常熟市兆恒众力精密机械有限公司 | Vacuum chamber and semiconductor processing equipment using same |
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