CN109868460B - Film growth system and growth method - Google Patents
Film growth system and growth method Download PDFInfo
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- CN109868460B CN109868460B CN201910193621.9A CN201910193621A CN109868460B CN 109868460 B CN109868460 B CN 109868460B CN 201910193621 A CN201910193621 A CN 201910193621A CN 109868460 B CN109868460 B CN 109868460B
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Abstract
The invention relates to a film growth system and a growth method, belonging to the field of material preparation; the sample room is connected with the central shaft through a cross rod and is used for transferring a sample in the sample room, and the transfer of the sample comprises transfer among the small chambers and/or transfer between the small chambers and the large chamber; the small chambers comprise a first small chamber, a second small chamber and an annealing chamber, and openable through holes are formed in the bottoms of the first small chamber and the second small chamber; the system provided by the invention has the functions of atomic layer deposition and annealing at the same time, can prepare a film with a larger difference between the source temperature and the reaction temperature of the sample adsorption precursor, and enlarges the application range of the atomic layer deposition equipment.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a film growth system and a film growth method.
Background
At present, the main methods for growing the thin film include physical methods and chemical methods, the physical methods mainly include vacuum evaporation, magnetron sputtering, ion plating and the like, and the chemical methods mainly include chemical vapor deposition, atomic layer deposition and the like. Atomic layer deposition is a method of depositing a thin film on the surface of a substrate by introducing a precursor source colloid into a cavity to perform a chemical reaction, and is mainly applied to semiconductors, photoelectric materials, integrated circuits, copper interconnection seed crystal layers and the like at present. The atomic layer deposition has the advantages of good shape retention and film thickness controllability, but the existing atomic layer deposition film is mainly amorphous, an annealing process is needed for converting the film into a crystalline film, and the annealing and the atomic layer deposition are often completed in different devices.
In the field of atomic layer deposition and annealing, chinese patent (201410454132.1) "atomic layer deposition equipment", the atomic layer deposition equipment includes a reaction chamber, an upper cover plate, a gas distributor, a valve group, a plurality of input and output ports, a process gas is communicated with an opening of the upper cover plate through the reaction chamber, the process gas can be retained less in a pipeline, while later-stage overhaul and maintenance are performed; chinese patent (201580080010609. X) "atomic layer deposition apparatus and atomic layer deposition system" supports a plurality of rectangular substrates together to form a thin film on the substrate surface by the relative rotation of gas injection, thereby reducing the installation space of the apparatus and significantly improving the production speed; chinese patent (201710887168.2) 'annealing device and annealing method' provides an annealing device, which comprises an annealing chamber, a conveying chamber, a lid and a conveying opening, wherein a substrate is annealed in the chamber, and the substrate is pumped by a vacuum pump continuously through a protective gas during the annealing process, so as to reduce the influence of external air entering the chamber on the substrate; the apparatus of U.S. Pat. No. 4, 20070134823, 1 "Atomic layer deposition apparatus and method" includes a separate chamber, gas supply line, gas exhaust line, and flow meter for detecting gas flow rate, which can precisely control the thickness of the film; the US patent (US 20100044932 a1) "Continuous annealing equipment" apparatus comprises a pre-heating zone, a soaking zone and a rapid cooling zone in which a gas jet cools the apparatus, each heating zone having a thermal sensor to control temperature.
At present, in the process of preparing a thin film, atomic layer deposition and annealing are usually completed in different devices respectively, there are crystalline state thin film growth deficiencies of the atomic layer deposition device, and the thin film is transferred to the annealing device at the later stage, which is easy to pollute a sample.
Disclosure of Invention
In view of the above technical problems, an object of the present invention is to provide a thin film growth system and a thin film growth method, in which the system integrates atomic layer deposition and annealing functions, thereby solving the technical problems of insufficient crystalline thin film growth and sample contamination caused by the fact that atomic layer deposition and annealing are respectively performed in different devices, and simultaneously solving the problem that the existing atomic layer deposition device cannot be used for thin film growth in which the difference between the source temperature of a sample adsorbing a precursor and the reaction temperature thereof is large.
The invention provides a film growth system, which comprises a sample chamber, a large chamber, a plurality of small chambers and a central shaft, wherein the small chambers are positioned in the large chamber, the central shaft is positioned in the center of the large chamber shaft, the sample chamber is connected with the central shaft through a cross rod and is used for transferring a sample in the sample chamber, and the transfer of the sample comprises the transfer among the small chambers and/or the transfer between the small chambers and the large chamber; the multiple small chambers comprise a first small chamber, a second small chamber and an annealing chamber, and openable through holes are formed in the bottoms of the first small chamber and the second small chamber and used for introducing precursors.
Further, the radius of rotation of the sample chamber along the central axis is equal to the distance from the small chamber to the central axis.
Furthermore, the film growth system further comprises a vacuum pump, wherein the vacuum pump is connected with the large chamber and the annealing chamber and used for vacuumizing the large chamber and the annealing chamber.
Further, the material of the large chamber and the small chamber comprises stainless steel or aluminum alloy.
The invention also provides a film growth method, which comprises the following steps:
s1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, heating the small chambers, and enabling the small chambers to be in a preset temperature state respectively;
s2, placing a sample chamber into a first small chamber, placing a sample into the sample chamber, filling the first small chamber with a first precursor, and performing saturation adsorption on the sample in the first precursor to obtain a first sample;
s3, transferring the sample chamber containing the first sample from the first small chamber to a large chamber through a central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling a second precursor into the second small chamber, and carrying out chemical reaction on the second precursor and the first precursor adsorbed on the surface of the sample to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber to the large chamber through the central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline film.
Further, in S2, the dissolution or melting temperature of the sample is greater than the growth temperature of the thin film.
Further, in S3 and S5, the inert gas includes at least one of argon, helium, and nitrogen; the inert gas is exhausted by a vacuum pump.
Further, in S4, the first film includes at least one of a nitride, an oxide, a simple metal, a sulfide, a carbide, a fluoride, a silicide, a group iii-v compound, and a group iv-v compound.
Further, by cyclically operating steps S1 to S5, a crystalline thin film of a target thickness is obtained.
In the present invention, the first film and the second film are both amorphous films.
Compared with the prior art, the invention has the following advantages:
1. the system provided by the invention has the functions of atomic layer deposition and annealing at the same time.
2. By utilizing the system provided by the invention, the sample cannot cause pollution, and the prepared crystalline film has sufficient growth.
3. The system and the method provided by the invention can be used for the growth of a film with a larger difference between the source temperature of the sample adsorbing the precursor and the reaction temperature of the sample adsorbing the precursor, and the application range of the atomic layer deposition equipment is expanded, so that the original film which is not suitable for atomic layer deposition can also be subjected to atomic layer deposition.
Drawings
FIG. 1 is a perspective view of a thin film growth system;
FIG. 2 is a top view of a thin film growth system;
wherein: 1. sample chamber, 2, big chamber, 3, little chamber, 31, first little chamber, 32, annealing room, 33, second little chamber, 4, center axis.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The invention provides a film growth system, which comprises a sample chamber, a large chamber, a plurality of small chambers and a central shaft, wherein the small chambers are positioned in the large chamber, the central shaft is positioned in the center of the large chamber shaft, the sample chamber is connected with the central shaft through a cross rod and is used for transferring a sample in the sample chamber, and the transfer of the sample comprises the transfer among the small chambers and/or the transfer between the small chambers and the large chamber; the multiple small chambers comprise a first small chamber, a second small chamber and an annealing chamber, and openable through holes are formed in the bottoms of the first small chamber and the second small chamber and used for introducing precursors.
The film growth system further comprises a vacuum pump, wherein the vacuum pump is connected with the large chamber and the annealing chamber and used for vacuumizing the large chamber and the annealing chamber.
The large chamber and the small chamber are made of stainless steel or aluminum alloy.
The invention also provides a film growth method, which comprises the following steps:
s1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, heating the small chambers, and enabling the small chambers to be in a preset temperature state respectively;
s2, placing a sample chamber into a first small chamber, placing a sample into the sample chamber, filling the first small chamber with a first precursor, and performing saturation adsorption on the sample in the first precursor to obtain a first sample;
s3, transferring the sample chamber containing the first sample from the first small chamber to a large chamber through a central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling a second precursor into the second small chamber, and carrying out chemical reaction on the second precursor and the first precursor adsorbed on the surface of the sample to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber to the large chamber through the central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline film.
In S2, the dissolution or melting temperature of the sample is greater than the growth temperature of the thin film.
S3 and S5, wherein the inert gas includes at least one of argon, helium and nitrogen; the inert gas is exhausted by a vacuum pump.
In S4, the first thin film includes at least one of a nitride, an oxide, a simple metal, a sulfide, a carbide, a fluoride, a silicide, a group iii-v compound, and a group iv-v compound.
By cyclically operating steps S1 to S5, a crystalline thin film of a target thickness is obtained.
Example 1
A thin film growth system comprising a sample chamber, a large chamber, a plurality of small chambers, a central shaft, said plurality of small chambers being located within said large chamber, said central shaft being located centrally of said large chamber shaft, said sample chamber being connected to said central shaft by a cross-bar for transferring a sample in said sample chamber, said transferring of said sample comprising transferring between said plurality of small chambers, and/or transferring between said small chambers and said large chamber; the multiple small chambers comprise a first small chamber, a second small chamber and an annealing chamber, and openable through holes are formed in the bottoms of the first small chamber and the second small chamber and used for introducing precursors.
Specifically, in order to transfer the sample in the sample chamber among a plurality of small chambers, the rotating radius of the sample chamber along the central axis is equal to the distance from the small chambers to the central axis, and the sample chamber can be rotated to the position above the small chambers, so that the samples in various stages in the sample chamber are processed in different small chambers.
Example 2
S1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, and heating the small chambers to enable the temperature of the first small chamber to be 100 ℃, the temperature of the second small chamber to be 300 ℃ and the temperature of the annealing chamber to be 800 ℃;
s2, placing the sample chamber into a first small chamber, placing a silicon wafer into the sample chamber, filling the first small chamber with a precursor trimethylaluminum, and performing saturated adsorption on the silicon wafer in the precursor trimethylaluminum to obtain a first sample;
s3, transferring the sample chamber filled with the first sample from the first small chamber to a large chamber through a central shaft, and introducing nitrogen into the large chamber for purging, wherein in the purging process, a vacuum pump discharges the nitrogen to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling ammonia gas serving as a precursor into the second small chamber, and carrying out chemical reaction on the ammonia gas and the trimethylaluminum adsorbed on the silicon surface to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber to the large chamber through the central shaft, introducing nitrogen into the large chamber for purging, and discharging the nitrogen in the purging process to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline aluminum nitride film.
By cyclically operating step S1 to step S5300 times, an aluminum nitride thin film of a target thickness is obtained.
Example 3
S1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, and heating the small chambers to enable the temperature of the first small chamber to be 80 ℃, the temperature of the second small chamber to be 130 ℃ and the temperature of the annealing chamber to be 500 ℃;
s2, placing the sample chamber into a first small chamber, placing quartz glass into the sample chamber, filling the first small chamber with a precursor of copper hexafluoroacetylacetonate, and performing saturation adsorption on the quartz glass on the precursor of copper hexafluoroacetylacetonate to obtain a first sample;
s3, transferring the sample chamber filled with the first sample from the first small chamber to a large chamber through a central shaft, introducing argon gas into the large chamber for purging, and discharging the argon gas through a vacuum pump in the purging process to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling the second small chamber with a precursor diethyl zinc, and carrying out chemical reaction on the diethyl zinc and the hexafluoroacetylacetone copper adsorbed on the surface of the quartz glass to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber into the large chamber through the central shaft, introducing argon into the large chamber for purging, and discharging the argon in the purging process to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline elemental copper film.
And obtaining the elemental copper film with the target thickness by circularly operating the step S1 to the step S5300.
Example 4
S1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, and heating the small chambers to enable the temperature of the first small chamber to be 100 ℃, the temperature of the second small chamber to be 300 ℃ and the temperature of the annealing chamber to be 800 ℃;
s2, placing the sample chamber into a first small chamber, placing a silicon wafer into the sample chamber, filling the first small chamber with a precursor tetra-dimethylamino-titanium, and performing saturated adsorption on the silicon wafer in the precursor tetra-dimethylamino-titanium to obtain a first sample;
s3, transferring the sample chamber filled with the first sample from the first small chamber into a large chamber through a central shaft, and introducing helium gas into the large chamber for purging, wherein in the purging process, a vacuum pump exhausts the helium gas to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling the second small chamber with precursor water, and carrying out chemical reaction on the water and the titanium tetra-dimethylamino adsorbed on the silicon surface to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber into the large chamber through the central shaft, introducing helium into the large chamber for purging, and discharging the helium in the purging process to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline titanium dioxide film.
By cyclically operating step S1 to step S5100 times, a titanium dioxide thin film of a target thickness is obtained.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (4)
1. A thin film growth method using a thin film growth system, the thin film growth system comprising a sample chamber, a large chamber, a plurality of small chambers, a central shaft, the plurality of small chambers being located within the large chamber, the central shaft being located at the center of the large chamber shaft, the sample chamber being connected to the central shaft by a cross bar for transferring a sample in the sample chamber, the transferring of the sample comprising transferring between the plurality of small chambers, and/or transferring between the small chambers and the large chamber; the film growth method comprises the following steps that:
s1, starting a vacuum pump to enable the large chamber and the annealing chamber to be in a vacuum state, heating the small chambers, and enabling the small chambers to be in a preset temperature state respectively;
s2, placing the sample chamber into a first small chamber, placing a sample into the sample chamber, filling the first small chamber with a first precursor, and performing saturation adsorption on the sample in the first precursor to obtain a first sample, wherein the dissolution or melting temperature of the sample is higher than the growth temperature of the film;
s3, transferring the sample chamber containing the first sample from the first small chamber to a large chamber through a central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second sample;
s4, transferring the sample chamber containing the second sample from the large chamber into a second small chamber through the central shaft, filling a second precursor into the second small chamber, and carrying out chemical reaction on the second precursor and the first precursor adsorbed on the surface of the sample to obtain a first film;
s5, transferring the sample chamber filled with the first film from the second small chamber to the large chamber through the central shaft, and introducing inert gas into the large chamber for purging, wherein in the purging process, the inert gas is discharged to obtain a second film;
and S6, transferring the sample chamber filled with the second film from the large chamber to an annealing chamber through the central shaft, and carrying out high-temperature annealing operation to obtain the crystalline film.
2. The thin film growth method as claimed in claim 1, wherein the inert gas includes at least one of argon, helium and nitrogen in S3 and S5, and the inert gas is exhausted by a vacuum pump.
3. The method of claim 1, wherein in S4, the first film includes at least one of nitride, oxide, elemental metal, sulfide, carbide, fluoride, silicide, a group iii-v compound, and a group iv compound.
4. The thin film growth method as claimed in claim 1, wherein the crystalline thin film of a target thickness is obtained by cyclically operating steps S1 to S5.
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| CN104233226A (en) * | 2013-06-09 | 2014-12-24 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Atomic layer deposition equipment |
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| CN106555174A (en) * | 2015-09-28 | 2017-04-05 | 超科技公司 | High production capacity multi-chamber atomic layer deposition system and method |
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Patent Citations (6)
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|---|---|---|---|---|
| CN102002685A (en) * | 2009-09-01 | 2011-04-06 | 东京毅力科创株式会社 | Film formation apparatus and film formation method |
| CN201901700U (en) * | 2010-09-17 | 2011-07-20 | 中微半导体设备(上海)有限公司 | MOCVD (metal-organic chemical vapor deposition) processing system realizing automatic substrate conveying |
| CN102534556A (en) * | 2012-02-20 | 2012-07-04 | 姜谦 | Normal-pressure multi-cavity atomic layer deposition equipment |
| CN104233226A (en) * | 2013-06-09 | 2014-12-24 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Atomic layer deposition equipment |
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