CN112159972A - In-situ monitoring atomic layer deposition equipment - Google Patents
In-situ monitoring atomic layer deposition equipment Download PDFInfo
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- CN112159972A CN112159972A CN202011159341.5A CN202011159341A CN112159972A CN 112159972 A CN112159972 A CN 112159972A CN 202011159341 A CN202011159341 A CN 202011159341A CN 112159972 A CN112159972 A CN 112159972A
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- 238000012544 monitoring process Methods 0.000 title claims abstract description 71
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 52
- 238000000231 atomic layer deposition Methods 0.000 title claims abstract description 42
- 238000000151 deposition Methods 0.000 claims abstract description 90
- 230000008021 deposition Effects 0.000 claims abstract description 89
- 238000010894 electron beam technology Methods 0.000 claims abstract description 85
- 239000002243 precursor Substances 0.000 claims abstract description 50
- 238000004891 communication Methods 0.000 claims description 18
- 238000010926 purge Methods 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 238000002128 reflection high energy electron diffraction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 25
- 239000010408 film Substances 0.000 description 18
- 239000010409 thin film Substances 0.000 description 13
- 230000008569 process Effects 0.000 description 11
- 238000005137 deposition process Methods 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 7
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000009304 pastoral farming Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
- C23C16/52—Controlling or regulating the coating process
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- Chemical & Material Sciences (AREA)
- 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 discloses an in-situ monitoring atomic layer deposition device, which comprises: a precursor supply unit; the deposition chamber is communicated with the precursor supply unit, and a sample stage is arranged in the deposition chamber; the first electron beam emission unit is communicated with the deposition chamber and emits a first electron beam to the sample stage; a second electron beam receiving unit communicating with the deposition chamber and receiving a second electron beam formed by diffraction from the sample stage; the first vacuum degree adjusting unit is communicated with the electron beam emitting unit; and; and the second vacuum degree adjusting unit is communicated with the deposition chamber. According to the method and the device, the in-situ monitoring atomic layer deposition equipment and the RHEED are independently arranged in the prior art, when monitoring is needed, the equipment needs to be built and assembled again, the building work is labor-consuming and time-consuming, the equipment environment built in the mode is difficult to guarantee the accuracy of the monitoring data, and the technical problem is solved.
Description
Technical Field
The invention relates to the technical field of thin film growth technology, in particular to in-situ monitoring atomic layer deposition equipment.
Background
The atomic layer deposition process is a self-limiting film growth process, and different precursors are introduced into the reaction chamber in turn for deposition, so that a film with good shape retention and low surface roughness can be obtained. In addition, the thickness of the thin film can be accurately controlled by controlling the introduction times of the precursor. In the initial stage of atomic layer deposition, no clear theoretical research is available on the adsorption reaction between the film and the substrate and between the film layers, and it is not clear in practical experiments which precursor is introduced to deposit the film, so that appropriate equipment is required for real-time and in-situ monitoring.
The reflection type high energy electron diffractometer (RHEED) is used for obtaining diffraction fringes and fringe intensity conditions on the surface of a thin film by striking an electron beam on the surface of a sample in a glancing incidence mode and striking the electron beam on a fluorescent screen after elastic scattering. The growth state, crystallinity, surface roughness, and the number of growth cycles of the thin film surface can be judged by analyzing the shape and intensity of the diffraction fringes. Because the electron beam is applied to the sample in a grazing incidence mode, the operation depth is only 1-2 atomic layers on the surface of the film, the film cannot be damaged, and nondestructive monitoring can be realized.
However, in-situ monitoring atomic layer deposition equipment and RHEED among the prior art are independently arranged, when monitoring is needed, re-construction and assembly are needed, the construction work is labor-consuming and time-consuming, and the equipment environment constructed in the mode is difficult to guarantee the accuracy of monitoring data.
Disclosure of Invention
The embodiment of the application provides an in-situ monitoring atomic layer deposition equipment, has solved in prior art in-situ monitoring atomic layer deposition equipment and RHEED independent setting, when needing to monitor, need build again, the equipment, it takes a lot of work and time to build work, and the equipment environment that this kind of mode was built is difficult to guarantee the technical problem of monitoring data's accuracy.
The application provides the following technical scheme through an embodiment of the application:
an in-situ monitoring atomic layer deposition apparatus comprising: a precursor supply unit; the deposition chamber is communicated with the precursor supply unit, and a sample stage is arranged in the deposition chamber; the first electron beam emission unit is communicated with the deposition chamber and emits a first electron beam to the sample stage; a second electron beam receiving unit communicating with the deposition chamber and receiving a second electron beam formed by diffraction from the sample stage; the first vacuum degree adjusting unit is communicated with the electron beam emitting unit; and; and the second vacuum degree adjusting unit is communicated with the deposition chamber.
In one embodiment, the electron beam emission unit comprises an electron gun and an electron gun duct, wherein one end of the electron gun duct is communicated with the electron gun through an electron gun gate valve, and the other end of the electron gun duct is communicated with the deposition chamber.
In one embodiment, the first vacuum degree adjusting unit includes: an electron difference unit in communication with the electron gun.
In one embodiment, the second vacuum degree adjusting unit includes: a third sub-conditioning unit in communication with the deposition chamber.
In one embodiment, the third sub-regulation unit includes: the device comprises a first mechanical pump, a first communication pipeline and a pre-pumping valve, wherein the pre-pumping valve is arranged on the first communication pipeline; the first mechanical pump is communicated with the deposition chamber through the first communication pipeline.
In one embodiment, the second vacuum degree adjusting unit further includes: and the fourth sub-regulation unit is communicated with the deposition chamber.
In one embodiment, the fourth sub-regulation unit includes: the system comprises a second mechanical pump, a second communicating pipeline, a turbomolecular pump, a third communicating pipeline, a high valve and a front valve, wherein the high valve is arranged on the second communicating pipeline, and the front valve is arranged on the third communicating pipeline; the second mechanical pump is also communicated with the turbo molecular pump through the third communicating pipeline, and the turbo molecular pump is communicated with the deposition chamber through a second communicating pipeline.
In one embodiment, the in-situ monitoring atomic layer deposition apparatus further comprises: and the gas filling pipeline is communicated with the deposition chamber and is used for providing purge gas for the deposition chamber.
In one embodiment, the precursor supply unit comprises: a plurality of precursor subunits, each of the precursor subunits in communication with the plenum.
In one embodiment, the electron beam receiving unit comprises a phosphor screen.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
in the in-situ monitoring atomic layer deposition equipment provided by the application, a precursor supply unit, a deposition chamber, an electron beam emission unit, an electron beam receiving unit, a first vacuum degree adjusting unit and a second vacuum degree adjusting unit are integrated together, when a thin film needs to be grown, firstly, the vacuum degree of the deposition chamber is adjusted through the second vacuum degree adjusting unit, so that the vacuum degree of the deposition chamber can reach the vacuum degree of deposition reaction, then, the precursor is supplied into the deposition chamber through the precursor supply unit, and the supplied precursor is subjected to deposition reaction on a sample table arranged in the deposition chamber to form the thin film; when in-situ monitoring is needed, the vacuum degree of the electron beam emission unit is adjusted through the first vacuum degree adjusting unit, so that the vacuum degree of the electron beam emission unit can reach the optimal in-situ monitoring vacuum state, at the moment, the electron beam emission unit is used for emitting a first electron beam to the sample stage, the electron beam receiving unit is used for receiving a second electron beam for in-situ monitoring, and because the interference of the first electron beam on air molecules in the environment is small, the diffraction stripe information for reflecting the growth condition of the film, which is obtained based on the second electron beam, is more accurate. Simultaneously, the atomic layer deposition function and normal position monitoring function have been integrateed to the in situ monitoring atomic layer deposition equipment of this application, when needing to monitor, need not to build again, consequently, in this application original position monitoring atomic layer deposition equipment and RHEED independent setting among the prior art have been solved, when needing to monitor, need build again, the equipment, it takes time and labor to build work, and the equipment environment that this kind of mode was built, is difficult to guarantee the technical problem of monitoring data's accuracy.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an in-situ monitoring atomic layer deposition apparatus according to an embodiment of the present disclosure.
Detailed Description
The embodiment of the application provides an in-situ monitoring atomic layer deposition equipment, has solved in prior art in-situ monitoring atomic layer deposition equipment and RHEED independent setting, when needing to monitor, need build again, the equipment, it takes a lot of work and time to build work, and the equipment environment that this kind of mode was built is difficult to guarantee the technical problem of monitoring data's accuracy.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
in the in-situ monitoring atomic layer deposition equipment provided by the application, a precursor supply unit, a deposition chamber, an electron beam emission unit, an electron beam receiving unit, a first vacuum degree adjusting unit and a second vacuum degree adjusting unit are integrated together, when a thin film needs to be grown, firstly, the vacuum degree of the deposition chamber is adjusted through the second vacuum degree adjusting unit, so that the vacuum degree of the deposition chamber can reach the vacuum degree of deposition reaction, then, the precursor is supplied into the deposition chamber through the precursor supply unit, and the supplied precursor is subjected to deposition reaction on a sample table arranged in the deposition chamber to form the thin film; when in-situ monitoring is needed, the vacuum degree of the electron beam emission unit is adjusted through the first vacuum degree adjusting unit, so that the vacuum degree of the electron beam emission unit can reach the optimal in-situ monitoring vacuum state, at the moment, the electron beam emission unit is used for emitting a first electron beam to the sample stage, the electron beam receiving unit is used for receiving a second electron beam for in-situ monitoring, and because the interference of the first electron beam on air molecules in the environment is small, the diffraction stripe information for reflecting the growth condition of the film, which is obtained based on the second electron beam, is more accurate. Simultaneously, the atomic layer deposition function and normal position monitoring function have been integrateed to the in situ monitoring atomic layer deposition equipment of this application, when needing to monitor, need not to build again, consequently, in this application original position monitoring atomic layer deposition equipment and RHEED independent setting among the prior art have been solved, when needing to monitor, need build again, the equipment, it takes time and labor to build work, and the equipment environment that this kind of mode was built, is difficult to guarantee the technical problem of monitoring data's accuracy.
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
Example one
As shown in fig. 1, the present embodiment provides an in-situ monitoring atomic layer deposition apparatus for forming a thin film on a substrate, the in-situ monitoring atomic layer deposition apparatus comprising: the system comprises a precursor supply unit, an inflation pipeline 5, a deposition chamber 7, an electron beam emission unit, an electron beam receiving unit, a first vacuum degree adjusting unit and a second vacuum degree adjusting unit, wherein the following units are respectively explained in detail as follows:
a gas charging pipe 5 communicated with the deposition chamber 7 for supplying a purge gas to the deposition chamber 7, wherein the purge gas may be a low activity gas, and is more commonly nitrogen N2. In the specific implementation process, the purge gas provided by the gas charging pipeline 5 can be used for purging the deposition chamber 7, can also be used as a carrier to carry in the precursor, and can also be used for stabilizing the vacuum degree of the deposition chamber 7.
And the precursor supply unit is used for supplying a precursor, and the precursor is a reactant for growing the thin film. In the specific implementation process, the precursor supply unit comprises a plurality of precursor subunits 6, each precursor subunit 6 stores one precursor participating in the reaction, each precursor subunit 6 is connected to the gas filling pipeline 5 through a valve, and the precursor stored in the precursor supply unit is driven by the purge gas to enter the deposition chamber 7.
And the deposition chamber 7 is communicated with the precursor supply unit, a sample table 71 is arranged in the deposition chamber 7, the sample table 71 is used for placing a substrate needing to grow a thin film, and the precursor introduced into the deposition chamber 7 is deposited on the substrate of the sample table 71.
And an electron beam emission unit, which is communicated with the deposition chamber 7, and is used for emitting a first electron beam to the sample stage 71, namely, emitting the first electron beam to the substrate film on the sample stage 71. In a specific implementation, the electron beam emitting unit may be disposed at an upper left or upper right position of the sample stage 71, so that the emitted first electron beam is directed toward the sample stage 71.
Further, the electron beam emission unit comprises an electron gun 1 and an electron gun pipeline 3, the electron gun 1 is used for emitting a first electron beam, one end of the electron gun pipeline 3 is communicated with the electron gun 1 through an electron gun gate valve 2, and the other end of the electron gun pipeline 3 is communicated with the deposition chamber 7 and used for guiding the first electron beam to a sample table 71 in the deposition chamber 7. In this embodiment, when in-situ monitoring is not required, the electron gun 1 is isolated from other regions by the electron gun gate valve 2, so as to prevent external impurity gases (e.g., precursors in the deposition process, impurity gases in the deposition chamber 7) from oxidizing the filament of the electron gun 1 and affecting the lifetime of the electron gun 1.
And the electron beam receiving unit is communicated with the deposition chamber 7 and is used for receiving a second electron beam formed by diffraction of the sample stage 71 on the first electron beam, namely receiving a second electron beam formed by diffraction of the substrate film on the sample stage 71.
In a specific implementation process, the electron beam receiving unit may be disposed at an upper left or upper right position of the sample stage 71, and corresponds to the disposed position of the electron beam emitting unit.
Further, the electron beam receiving unit comprises a fluorescent screen 9 and a fluorescent screen gate valve 8, in the embodiment, when in-situ monitoring is not needed, the fluorescent screen 9 is separated from other areas by the fluorescent screen gate valve 8, so that the phenomenon that external impurity gas is deposited on the fluorescent screen 9 to influence the collection of the second electron beam and further influence the accuracy of data collection is avoided.
And the first vacuum degree adjusting unit is communicated with the electron beam emitting unit.
The first vacuum degree adjusting unit is used for adjusting the vacuum degree of the electron beam emission unit, so that the vacuum degree of the electron beam emission unit can be adjusted to a lower state, and the phenomenon that the filament of the electron beam emission unit is oxidized due to the existence of impurity gas in the electron beam emission unit, and the service life of the electron beam emission unit is further influenced can be avoided; meanwhile, the impurity gas can be prevented from colliding with electrons of the first electron beam, so that the electron track of the first electron beam is changed, the interference of air molecules on the first electron beam is reduced, and the subsequent diffraction stripe information obtained based on the second electron beam and used for reflecting the growth condition of the film is more accurate.
In a specific implementation process, the first vacuum degree adjusting unit includes an electronic differential unit, which includes a first sub-adjusting unit 41 and a second sub-adjusting unit 42, wherein,
a first sub-adjusting unit 41, which is communicated with one end of the electron gun 1 far away from the electron gun pipeline 3;
and a second sub-adjustment unit 42 communicating with an end of the electron gun 1 near the electron gun tube 3.
In this embodiment, the first sub-adjusting unit 41 may adjust the vacuum degree of the end of the electron gun 1 away from the electron gun tube 3 to a first predetermined vacuum degree before the in-situ monitoring, where the first predetermined vacuum degree is a vacuum value required for the in-situ monitoring, and as an example, the first predetermined vacuum degree is 5 × 10-7torr; the second sub-adjustment unit 42 may adjust the vacuum level at the end remote from the electron gun tube 3 to smoothly transition the vacuum level of the electron gun 1 to the deposition chamber 7 before in-situ monitoring.
And a second vacuum degree adjusting unit communicated with the deposition chamber 7 for adjusting the vacuum degree of the deposition chamber 7.
As an alternative embodiment, the second vacuum degree adjusting unit includes:
and the third sub-adjusting unit is communicated with the deposition chamber 7 and is used for adjusting the vacuum degree of the deposition chamber 7 to a second preset vacuum degree, wherein the second preset vacuum degree is a vacuum value required by deposition of the precursor.
Specifically, the degree of vacuum of the deposition chamber 7 may be first adjusted to a lower vacuum state by the third sub-adjustment unit, as one example, 5 × 10-3torr, at which the impurity gas in the deposition chamber 7 is substantially purged, and then, the degree of vacuum of the deposition chamber 7 may be adjusted to a second predetermined degree of vacuum by the purge gas supplied through the gas filling line 5, so as to adjust the degree of vacuum of the deposition chamber 7 to a vacuum value required for depositing the precursor, as an example, the second predetermined degree of vacuum is 0.2 torr.
As an example, the third sub-adjusting unit includes: the device comprises a first mechanical pump 14, a first communication pipeline and a pre-pumping valve 11, wherein the pre-pumping valve 11 is arranged on the first communication pipeline; and a first mechanical pump 14 communicating with the deposition chamber 7 through a first communication pipe.
Further, the second vacuum degree adjusting unit further includes:
a fourth sub-adjustment unit, which is communicated with the deposition chamber 7, and is configured to adjust the vacuum degree of the deposition chamber 7 to a third preset vacuum degree, where the third preset vacuum degree is a vacuum value required for performing in-situ monitoring, and as an example, the third preset vacuum degree is 5 × 10-7torr。
In this embodiment, through the regulation of fourth sub-regulation unit, can adjust the vacuum degree of deposition chamber 7 to third preset vacuum degree, thereby can adjust the vacuum degree in deposition chamber 7 to lower state, can avoid deposition chamber 7 to exist impurity gas, collide with the electron of first electron beam, thereby change the electron orbit of first electron beam, and then reduce the interference that first electron beam received air molecule, make the subsequent diffraction stripe information that is used for reacting the film growth situation based on that the second electron beam obtained more accurate.
As an example, the fourth sub-adjusting unit includes: a second mechanical pump 14, a second communication conduit, a turbomolecular pump 12, a third communication conduit, a high valve 10, and a pre-valve 13, wherein,
the high valve 10 is arranged on the second communicating pipeline, and the preceding valve 13 is arranged on the third communicating pipeline;
the second mechanical pump 14 is also communicated with the turbomolecular pump 12 through a third communication conduit, and the turbomolecular pump 12 is communicated with the deposition chamber 7 through a second communication conduit.
In this embodiment, the mechanical pump 14 is first used to reduce the high vacuum degree to avoid the impact of the high vacuum degree on the turbomolecular pump 12 and the influence on the service life of the turbomolecular pump, and then the turbomolecular pump 12 with high power is used to adjust the vacuum degree of the deposition chamber 7 to be as small as possible. In actual practice, the second mechanical pump 14 and the first mechanical pump 14 are implemented using the same mechanical pump.
The working principle and the working process of the in-situ monitoring atomic layer deposition apparatus according to the above embodiments are further described below by taking a process of growing a molybdenum disulfide (MoS2) film as an example, so that those skilled in the art can understand the working principle and the working process. It should be noted that the following examples are provided to assist those skilled in the art in understanding the above embodiments, and should not be construed as limiting the features of the in-situ monitoring atomic layer deposition apparatus provided herein.
First, preparation work for the deposition process is performed:
molybdenum precursor MoF is prepared in two precursor subunits 6 respectively6Sulfur precursor H2S, and all the components are kept at room temperature;
mixing Si/SiO2The substrate is placed into acetone, ethanol and deionized water for ultrasonic cleaning, and is placed on a sample table 71 of the deposition chamber 7 after being dried;
the mechanical pump and the pre-pump valve 11 are opened to pump the vacuum degree of the deposition chamber 7 to 5X 10-3torr to exhaust the impurity gas of the deposition chamber 7;
heating the cavity of the deposition chamber 7 to 250 ℃, and preserving the heat for one hour; heating the gas-filled pipeline 5 to 100-150 ℃ to ensure that the precursor is not adsorbed on the pipeline due to temperature reduction in the gas-filled pipeline 5;
the purge gas N is introduced through the gas charging pipeline 52Until the degree of vacuum of the deposition chamber 7 was 0.2torr, the preparation of the experimental conditions was completed.
Secondly, starting the deposition process of the atomic layer:
MoS2the film growth process is mainly divided into 6 steps: with N2Introducing a molybdenum precursor MoF as a carrier gas6Reacting and purging; then, the sulfur precursor H was introduced with N2 as a carrier gas2S, reacting and purging, wherein the cycle is a complete cycle of atomic layer deposition, and the required film thickness can be accurately controlled by controlling different cycle times.
Then, preparation of in-situ monitoring is performed (taking stopping the deposition process after each cycle is completed as an example, it should be noted that the time node of in-situ monitoring may be performed at any time during the process of not stopping the deposition process, or may be performed after stopping the deposition process after each growth cycle is performed during the deposition process):
when the primary circulation is finished, stopping the deposition process, and closing the gas-filled pipeline 5, the pre-pumping valve 11 and the mechanical pump in advance;
the former valve 13, the high valve 10 and the turbo molecular pump 12 are opened in this order, and the vacuum degree of the deposition chamber 7 is evacuated to 5X 10- 7torr; and opening the electron difference unit to pump the vacuum degree of the electron gun 1 to 5 × 10-7torr。
Then, an in-situ monitoring process is performed:
the vacuum condition is stabilized at 5 x 10-7RHEED monitoring is carried out after the torr, an electron gun gate valve 2 and a fluorescent screen gate valve 8 are opened, and an electron gun 1 emits a first electron beam to a sample film of a sample table 71 and reaches a fluorescent screen 9 after elastic scattering; the CCD behind the fluorescent screen 9 can monitor the information of the sample such as diffraction fringes, fringe intensity and the like.
Finally, after the monitoring is finished, closing the electron gun gate valve 2 and the fluorescent screen gate valve 8, then closing the high valve 10 and the pre-valve 13 in sequence, and opening the pre-pumping valve 11 and the inflation pipeline 5; and (4) continuing to deposit after the vacuum degree of the chamber is stabilized at 0.2torr, and only repeating the steps when monitoring is carried out again.
The technical scheme in the embodiment of the application at least has the following technical effects or advantages:
in the in-situ monitoring atomic layer deposition equipment provided by the application, a precursor supply unit, a deposition chamber, an electron beam emission unit, an electron beam receiving unit, a first vacuum degree adjusting unit and a second vacuum degree adjusting unit are integrated together, when a thin film needs to be grown, firstly, the vacuum degree of the deposition chamber is adjusted through the second vacuum degree adjusting unit, so that the vacuum degree of the deposition chamber can reach the vacuum degree of deposition reaction, then, the precursor is supplied into the deposition chamber through the precursor supply unit, and the supplied precursor is subjected to deposition reaction on a sample table arranged in the deposition chamber to form the thin film; when in-situ monitoring is needed, the vacuum degree of the electron beam emission unit is adjusted through the first vacuum degree adjusting unit, so that the vacuum degree of the electron beam emission unit can reach the optimal in-situ monitoring vacuum state, at the moment, the electron beam emission unit is used for emitting a first electron beam to the sample stage, the electron beam receiving unit is used for receiving a second electron beam for in-situ monitoring, and because the interference of the first electron beam on air molecules in the environment is small, the diffraction stripe information for reflecting the growth condition of the film, which is obtained based on the second electron beam, is more accurate. Simultaneously, the atomic layer deposition function and normal position monitoring function have been integrateed to the in situ monitoring atomic layer deposition equipment of this application, when needing to monitor, need not to build again, consequently, in this application original position monitoring atomic layer deposition equipment and RHEED independent setting among the prior art have been solved, when needing to monitor, need build again, the equipment, it takes time and labor to build work, and the equipment environment that this kind of mode was built, is difficult to guarantee the technical problem of monitoring data's accuracy.
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 (10)
1. An in-situ monitoring atomic layer deposition apparatus, comprising:
a precursor supply unit;
the deposition chamber is communicated with the precursor supply unit, and a sample stage is arranged in the deposition chamber;
the first electron beam emission unit is communicated with the deposition chamber and emits a first electron beam to the sample stage;
a second electron beam receiving unit communicating with the deposition chamber and receiving a second electron beam formed by diffraction from the sample stage;
a first vacuum degree adjusting unit communicated with the electron beam emitting unit, and;
and the second vacuum degree adjusting unit is communicated with the deposition chamber.
2. The in-situ monitoring atomic layer deposition apparatus according to claim 1, wherein the electron beam emission unit comprises an electron gun and an electron gun tube, wherein,
one end of the electron gun pipeline is communicated with the electron gun through an electron gun gate valve, and the other end of the electron gun pipeline is communicated with the deposition chamber.
3. The in-situ monitoring atomic layer deposition apparatus of claim 2, wherein the first vacuum level adjustment unit comprises:
an electron difference unit in communication with the electron gun.
4. The in-situ monitoring atomic layer deposition apparatus of claim 1, wherein the second vacuum level adjustment unit comprises:
a third sub-conditioning unit in communication with the deposition chamber.
5. The in-situ monitoring atomic layer deposition apparatus according to claim 4, wherein the third sub-conditioning unit comprises: a first mechanical pump, a first communicating pipeline and a pre-pumping valve, wherein,
the pre-pumping valve is arranged on the first communication pipeline;
the first mechanical pump is communicated with the deposition chamber through the first communication pipeline.
6. The in-situ monitoring atomic layer deposition apparatus of claim 1, wherein the second vacuum level adjustment unit further comprises:
and the fourth sub-regulation unit is communicated with the deposition chamber.
7. The in-situ monitoring atomic layer deposition apparatus according to claim 6, wherein the fourth sub-conditioning unit comprises: a second mechanical pump, a second communicating pipeline, a turbo molecular pump, a third communicating pipeline, a high valve and a front valve,
the high valve is arranged on the second communicating pipeline, and the front valve is arranged on the third communicating pipeline;
the second mechanical pump is also communicated with the turbo molecular pump through the third communicating pipeline, and the turbo molecular pump is communicated with the deposition chamber through a second communicating pipeline.
8. The in-situ monitoring atomic layer deposition apparatus according to claim 1, further comprising:
and the gas filling pipeline is communicated with the deposition chamber and is used for providing purge gas for the deposition chamber.
9. The in-situ monitoring atomic layer deposition apparatus according to claim 8, wherein the precursor supply unit comprises:
a plurality of precursor subunits, each of the precursor subunits in communication with the plenum.
10. The in-situ monitoring atomic layer deposition apparatus of claim 1, wherein the electron beam receiving unit includes a phosphor screen.
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