CN114592180A - Preparation method of magnesium fluoride film and related equipment - Google Patents
Preparation method of magnesium fluoride film and related equipment Download PDFInfo
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- CN114592180A CN114592180A CN202210224187.8A CN202210224187A CN114592180A CN 114592180 A CN114592180 A CN 114592180A CN 202210224187 A CN202210224187 A CN 202210224187A CN 114592180 A CN114592180 A CN 114592180A
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- 229910001635 magnesium fluoride Inorganic materials 0.000 title claims abstract description 77
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 77
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 66
- 239000011777 magnesium Substances 0.000 claims abstract description 66
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 55
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 53
- 239000011737 fluorine Substances 0.000 claims abstract description 53
- 238000010926 purge Methods 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 239000010408 film Substances 0.000 claims description 53
- 239000007789 gas Substances 0.000 claims description 31
- 239000010409 thin film Substances 0.000 claims description 28
- 238000004590 computer program Methods 0.000 claims description 23
- 238000003860 storage Methods 0.000 claims description 18
- BVUYFWJPRKTFKI-UHFFFAOYSA-N C(C)C=1C(C=CC=1)([Mg])CC Chemical compound C(C)C=1C(C=CC=1)([Mg])CC BVUYFWJPRKTFKI-UHFFFAOYSA-N 0.000 claims description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 13
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910052594 sapphire Inorganic materials 0.000 claims description 8
- 239000010980 sapphire Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- AKTIAGQCYPCKFX-FDGPNNRMSA-L magnesium;(z)-4-oxopent-2-en-2-olate Chemical compound [Mg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AKTIAGQCYPCKFX-FDGPNNRMSA-L 0.000 claims description 3
- OQWBVEQWPPRAMU-UHFFFAOYSA-L magnesium;7,7-dimethyloctanoate Chemical compound [Mg+2].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O OQWBVEQWPPRAMU-UHFFFAOYSA-L 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 11
- 238000010586 diagram Methods 0.000 description 14
- 230000003287 optical effect Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 238000012545 processing Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000006870 function Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000005234 chemical deposition Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- CKTALQCEAJJSTQ-UHFFFAOYSA-L [Mg+2].CP([O-])=O.CP([O-])=O Chemical compound [Mg+2].CP([O-])=O.CP([O-])=O CKTALQCEAJJSTQ-UHFFFAOYSA-L 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
-
- 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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
-
- 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]
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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)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The application discloses a preparation method of a magnesium fluoride film and related equipment, relates to the technical field of films, and can improve the film thickness uniformity in the process of preparing a large-area magnesium fluoride film. The preparation method of the magnesium fluoride film comprises the following steps: transferring the substrate to an atomic layer deposition reaction chamber; under the condition that the atomic layer deposition reaction chamber reaches the preparation condition, introducing a magnesium source into the atomic layer deposition reaction chamber and then performing gas purging on the atomic layer deposition reaction chamber; and after a fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber.
Description
Technical Field
The application relates to the technical field of films, in particular to a preparation method of a magnesium fluoride film and related equipment.
Background
MgF2(magnesium fluoride) is a colorless tetragonal crystal or powder, rutile-type lattice. Magnesium fluoride is an important optical material, particularly crystal high-purity magnesium fluoride, has a plurality of excellent properties, and the application field of the magnesium fluoride is more and more extensive. The magnesium fluoride film is prepared by magnesium hydroxide fluorination, thermal evaporation, PLD (laser pulse deposition), reactive magnetron sputtering, chemical deposition and the like.
However, the current preparation method can only carry out small-area coating, and the uniformity of the film thickness is difficult to control in the preparation process of large-area magnesium fluoride films.
Disclosure of Invention
The embodiment of the application provides a preparation method of a magnesium fluoride film and related equipment, which can improve the film thickness uniformity in the process of preparing a large-area magnesium fluoride film.
In a first aspect of the embodiments of the present application, a method for preparing a magnesium fluoride thin film is provided, including:
transferring the substrate to an atomic layer deposition reaction chamber;
under the condition that the atomic layer deposition reaction chamber reaches the preparation condition, introducing a magnesium source into the atomic layer deposition reaction chamber and then performing gas purging on the atomic layer deposition reaction chamber;
and after a fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber.
In some embodiments, the method for preparing a magnesium fluoride thin film further comprises:
and after the fluorine source is introduced into the atomic layer deposition reaction chamber for the set times and the gas purging is completed, controlling the atomic layer deposition reaction chamber to be cooled to the room temperature to obtain the magnesium fluoride film.
In some embodiments, the single pass of the magnesium source is in the range of 0.001 to 5 seconds, the single pass of the fluorine source is in the range of 0.001 to 10 seconds, and the single gas purge is in the range of 1 to 180 seconds.
In some embodiments, the preparation conditions of the ald reaction chamber include the substrate being heated to 25-500 ℃ in the ald reaction chamber, the pipe to which the ald reaction chamber is connected being heated to 25-200 ℃, the ald reaction chamber having a temperature in the range of 25-200 ℃ and the magnesium source and the fluorine source having a temperature in the range of 25-200 ℃.
In some embodiments, the substrate comprises silicon, sapphire, or glass;
the magnesium source comprises at least one of magnesium neodecanoate, magnesium 2,2,6, 6-tetramethyl-3, 5-heptanedionate, magnesium trifluoroacetylacetonate, magnesium hexafluoroacetylacetonate, magnesium acetylacetonate, magnesium metallocenes and bis-ethylcyclopentadienyl magnesium;
the fluorine source includes at least one of elemental fluorine and hydrogen fluoride.
In some embodiments, in the case where the substrate is sapphire, the magnesium source is bis-ethylcyclopentadienyl magnesium, and the fluorine source is hydrogen fluoride, the preparation conditions of the atomic layer deposition reaction chamber are:
the substrate is heated to 100 ℃, the temperature of the atomic layer deposition reaction chamber is 100 ℃, a pipeline connected with the atomic layer deposition reaction chamber is heated to 100 ℃, the temperature range of the magnesium source is 60-100 ℃, and the temperature of the fluorine source is 25 ℃.
In some embodiments, where the magnesium source is bis-ethylcyclopentadienyl magnesium and the fluorine source is hydrogen fluoride, the magnesium source is passed for a time period in the range of 0.5 to 1.2s, the fluorine source is passed for a time period in the range of 2 to 8s, and the gas purge is passed for a time period in the range of 20 to 60 s.
In some embodiments, the gas used for the gas purge comprises at least one of an inert gas and nitrogen.
In a second aspect of the embodiments of the present application, there is provided an electronic device, including:
a memory having a computer program stored therein;
a processor for implementing the method of preparing a magnesium fluoride thin film according to the first aspect when executing the computer program.
In a third aspect of the embodiments of the present application, a computer-readable storage medium is provided, where a computer program is stored on the computer-readable storage medium, and when the computer program is executed by a processor, the method for preparing a magnesium fluoride thin film according to the first aspect is implemented.
The preparation method of the magnesium fluoride film and the related equipment provided by the embodiment of the application adopt the atomic layer deposition mode to prepare the magnesium fluoride film, are self-limiting surface growth modes, and can realize the accurate control of the film thickness in the single atomic layer magnitude and the uniform conformal film coverage on the three-dimensional nano structure. The method for depositing the magnesium fluoride film by adopting the atomic layer deposition technology can be compatible with the existing optical device production line, is suitable for large-scale production, realizes the production of large-curvature optical devices, and can improve the film thickness uniformity in the process of preparing large-area magnesium fluoride films.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a magnesium fluoride thin film according to an embodiment of the present disclosure;
fig. 2 is a schematic structural diagram of a magnesium fluoride film prepared by a method for preparing a magnesium fluoride film according to an embodiment of the present disclosure;
fig. 3 is a schematic structural block diagram of an electronic device according to an embodiment of the present application;
fig. 4 is a schematic structural block diagram of a computer-readable storage medium according to an embodiment of the present application.
Detailed Description
In order to better understand the technical solutions provided by the embodiments of the present specification, the technical solutions of the embodiments of the present specification are described in detail below with reference to the drawings and specific embodiments, and it should be understood that the specific features in the embodiments and examples of the present specification are detailed descriptions of the technical solutions of the embodiments of the present specification, and are not limitations on the technical solutions of the embodiments of the present specification, and the technical features in the embodiments and examples of the present specification may be combined with each other without conflict.
In this document, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, 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. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element. The term "two or more" includes the case of two or more.
Magnesium fluoride is a colorless tetragonal crystal or powder, rutile-type lattice. Magnesium fluoride is an important optical material, particularly crystal high-purity magnesium fluoride, has a plurality of excellent properties, and the application field of the magnesium fluoride is more and more extensive. The preparation method of the magnesium fluoride film at present comprises a magnesium hydroxide fluorination method, a thermal evaporation method, a PLD (laser pulse deposition), a reactive magnetron sputtering method, a chemical deposition method and the like. However, the current preparation method can only carry out small-area coating, and the uniformity of the film thickness is difficult to control in the preparation process of large-area magnesium fluoride films.
In view of the above, embodiments of the present disclosure provide a method and related apparatus for preparing a magnesium fluoride thin film, which can improve the uniformity of the thickness of the magnesium fluoride thin film during the preparation of a large area.
In a first aspect of an embodiment of the present application, a method for preparing a magnesium fluoride thin film is provided, and fig. 1 is a schematic flow chart of the method for preparing a magnesium fluoride thin film provided in the embodiment of the present application. As shown in fig. 1, a method for preparing a magnesium fluoride thin film provided in an embodiment of the present application includes:
s100: the substrate is transferred to an atomic layer deposition reaction chamber. The substrate may be used as a deposition carrier for the magnesium fluoride thin film, and for example, the prepared substrate may be transferred to the ald reaction chamber by using a transfer robot, which is not limited in this embodiment.
S200: and under the condition that the atomic layer deposition reaction chamber reaches the preparation condition, introducing a magnesium source into the atomic layer deposition reaction chamber and then performing gas purging on the atomic layer deposition reaction chamber. The atomic layer deposition technology can be used for preparing films, film devices and the like in the field of microelectronics, and a magnesium source can be introduced into an atomic layer deposition reaction chamber in a gaseous form. Illustratively, a magnesium source is filled into a solid source heating source bottle of the atomic layer deposition equipment in a glove box, the heating temperature of the source bottle is set to heat the magnesium source until the vapor pressure of each pulse is stable, and in the case of the magnesium source being the bis-ethyl cyclopentadienyl magnesium, the bis-ethyl cyclopentadienyl magnesium is solid at room temperature and has lower saturated vapor pressure, so the bis-ethyl cyclopentadienyl magnesium needs to be heated to 60-100 ℃ by a solid source heating device of the atomic layer deposition equipment; so as to ensure that the diethyl cyclopentadienyl magnesium has enough vapor pressure pulse to enter a carrier gas system and is finally conveyed to the reaction chamber by the carrier gas. The gas purging can accelerate the homogenization of the magnesium source, and the magnesium source can be uniformly distributed in the atomic layer deposition reaction chamber, so that the magnesium is uniformly deposited on the surface of the substrate to form a uniform magnesium film.
S300: and after the fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber. Illustratively, the fluorine source can be introduced into the atomic layer deposition reaction chamber in a gas form, and the gas purging can accelerate the homogenization of the fluorine source, so that the fluorine source can be uniformly distributed in the atomic layer deposition reaction chamber, and the fluorine can be uniformly deposited on the surface of the substrate to form a uniform fluorine film.
The preparation method of the magnesium fluoride film provided by the embodiment of the application adopts an atomic layer deposition mode to prepare the magnesium fluoride film, is a self-limiting surface growth mode, and can realize the accurate controllability of the film thickness in the single atomic layer magnitude and the uniform conformal film coverage of 100% on a three-dimensional nano structure. The method for depositing the magnesium fluoride film by adopting the atomic layer deposition technology can be compatible with the existing optical device production line, is suitable for large-scale production, realizes the production of large-curvature optical devices, and can improve the film thickness uniformity in the process of preparing large-area magnesium fluoride films.
In some embodiments, the method for preparing a magnesium fluoride thin film of the present application further includes:
and after the fluorine source is introduced into the atomic layer deposition reaction chamber for the set times and the gas purging is completed, controlling the atomic layer deposition reaction chamber to cool to the room temperature to obtain the magnesium fluoride film. In the preparation process of the magnesium fluoride film, the number of times of introducing the magnesium source can be counted, the number of times of introducing the fluorine source is counted, after the fluorine source is introduced every time and gas purging is completed, whether the number of times of introducing the fluorine source reaches the set number of times is judged, if the number of times of introducing the fluorine source reaches the set number of times, the magnesium source is stopped to be continuously introduced, and the temperature of the atomic layer deposition reaction chamber is reduced to the room temperature to obtain the magnesium fluoride film. If the introduction times of the fluorine source do not reach the set times, the magnesium source is continuously introduced, and the magnesium source and the fluorine source are alternately introduced. In some embodiments, the introduction of the magnesium source may also be counted, and for example, fig. 2 is a schematic structural diagram of a magnesium fluoride film prepared by the method for preparing a magnesium fluoride film provided in the examples of the present application. As shown in fig. 2, the magnesium fluoride film includes 4 magnesium atomic layers and 3 fluorine atomic layers, the magnesium atomic layers are a first magnesium atomic layer Mg1, a second magnesium atomic layer Mg2, a third magnesium atomic layer Mg3 and a fourth magnesium atomic layer Mg4, the fluorine atomic layers are a first fluorine atomic layer F1, a second fluorine atomic layer F2 and a third fluorine atomic layer F3, and the number of times of introducing the magnesium source is 4.
According to the preparation method of the magnesium fluoride thin film, the magnesium source and the fluorine source are alternately introduced until the fluorine source is introduced for the set times, the preparation of the thin film can be stopped, and the magnesium fluoride thin film with uniform film thickness is obtained.
In some embodiments, the single pass of the magnesium source is in the range of 0.001 to 5 seconds, the single pass of the fluorine source is in the range of 0.001 to 10 seconds, and the single gas purge is in the range of 1 to 180 seconds. Illustratively, the gas used for the gas purge includes at least one of an inert gas and nitrogen. The substrate comprises silicon, sapphire or glass; the magnesium source comprises at least one of magnesium neodecanoate, magnesium 2,2,6, 6-tetramethyl-3, 5-heptanedionate (dimagnesium), magnesium trifluoroacetylacetonate, magnesium hexafluoroacetylacetonate (magnesium methylphosphinate), magnesium acetylacetonate, magnesium metallocenes, and magnesium diethylcyclopentadienyl; the fluorine source includes at least one of elemental fluorine and hydrogen fluoride.
In some embodiments, the atomic layer deposition reaction chamber is prepared under conditions including heating the substrate to 25-500 ℃ in the atomic layer deposition reaction chamber, heating the pipe to which the atomic layer deposition reaction chamber is connected to 25-200 ℃, the atomic layer deposition reaction chamber having a temperature in a range of 25-200 ℃, and the magnesium source and the fluorine source having a temperature in a range of 25-200 ℃. The pipeline connected to the ald reaction chamber may be a pipeline for introducing a magnesium source and a fluorine source, and the embodiment of the present application is not particularly limited.
In some embodiments, in the case where the substrate is sapphire, the magnesium source is bis-ethylcyclopentadienyl magnesium, and the fluorine source is hydrogen fluoride, the atomic layer deposition reaction chamber is prepared under the following conditions: the substrate is heated to 100 ℃, the temperature of the atomic layer deposition reaction chamber is 100 ℃, a pipeline connected with the atomic layer deposition reaction chamber is heated to 100 ℃, the temperature of the magnesium source ranges from 60 ℃ to 100 ℃, and the temperature of the fluorine source is 25 ℃.
Illustratively, the preparation method of the magnesium fluoride thin film provided by the embodiment of the present application includes the following steps:
and placing a substrate such as silicon, sapphire or glass in the atomic layer deposition reaction chamber by controlling the conveying mechanical arm, vacuumizing the atomic layer deposition reaction chamber and heating the substrate, the chamber, the pipeline, the reaction source and the like.
And when the cavity, the substrate, the pipeline, the reaction source and the like are heated and stabilized at a specific temperature, introducing a magnesium source for 0.001-5s, purging with gas for 1-180s, introducing a fluorine source for 0.001-10s, and purging with gas for 1-180s into the atomic layer deposition reaction cavity so as to perform atomic layer deposition in the cavity, and circulating for a set number of times to obtain the magnesium fluoride film.
After the magnesium fluoride film is deposited, the substrate is naturally cooled to room temperature in vacuum and then taken out, wherein the room temperature is usually 25 ℃.
The obtained uniform magnesium fluoride film is put in a vacuum drying oven for standby.
In some embodiments, where the magnesium source is bis-ethylcyclopentadienyl magnesium and the fluorine source is hydrogen fluoride, the magnesium source is passed for a time period in the range of 0.5 to 1.2s, the fluorine source is passed for a time period in the range of 2 to 8s, and the gas purge is passed for a time period in the range of 20 to 60 s.
Illustratively, the transfer robot is controlled to place the sapphire substrate in the ald reaction chamber, evacuate the ald reaction chamber and begin heating.
The method comprises the following steps of (1) filling the bis-ethyl cyclopentadienyl magnesium into a solid source heating source bottle of the atomic layer deposition equipment in a glove box, setting the heating temperature of the source bottle to heat a magnesium source until the vapor pressure of each pulse is stable, wherein the bis-ethyl cyclopentadienyl magnesium is solid at room temperature and has lower saturated vapor pressure, so that the bis-ethyl cyclopentadienyl magnesium needs to be heated to 60-100 ℃ by a solid source heating device of the atomic layer deposition equipment; so as to ensure that the diethyl cyclopentadienyl magnesium has enough vapor pressure pulse to enter a carrier gas system and is finally conveyed to the atomic layer deposition reaction chamber by the carrier gas. Since the hydrogen fluoride is gaseous at room temperature, the hydrogen fluoride is directly conveyed to the atomic layer deposition reaction chamber by the carrier gas.
When the temperature of the substrate reaches the preset value of 100-:
the first pulse is a bisethylcyclopentadienyl magnesium pulse, and the pulse time is 0.001-5 s; the pulse time of nitrogen purging is 20-60 s; the pulse time of the hydrogen fluoride is 2-8 s; the nitrogen purge pulse time was 20-60 s. The flow rates of the bisethylcyclopentadienyl magnesium and the hydrogen fluoride carrier gas were 45sccm, and the flow rates of the nitrogen gas in the other source lines were all set to 30 sccm. The growth thickness is 800 cycles of the above steps, i.e. the setting number is 200-.
According to the preparation method of the magnesium fluoride film, the magnesium fluoride film is deposited by the atomic layer deposition technology, the method is simple to operate, and mass production and compatibility with the existing optical device are facilitated; the magnesium fluoride film prepared by the atomic layer deposition method has good three-dimensional shape retention, and the thickness of the film is accurately controllable in the single atomic layer level. The method has important significance for the application of the magnesium fluoride film in the fields of optical lenses, photoelectric devices, optical devices, large-curvature devices and the like.
In a second aspect of the embodiments of the present application, an electronic device is provided, and fig. 3 is a schematic structural block diagram of the electronic device provided in the embodiments of the present application. As shown in fig. 3, an electronic device provided in an embodiment of the present application includes:
a memory 400, the memory 400 having stored therein a computer program;
a processor 500, the processor 500 being adapted to execute a computer program to implement the method for preparing a magnesium fluoride thin film according to the first aspect.
The preparation method of the magnesium fluoride film comprises the following steps:
the substrate is transferred to an atomic layer deposition reaction chamber.
And under the condition that the atomic layer deposition reaction chamber reaches the preparation condition, introducing a magnesium source into the atomic layer deposition reaction chamber and then performing gas purging on the atomic layer deposition reaction chamber.
And after the fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber.
It should be noted that the electronic device may be a controller, and the controller may be disposed in the atomic layer deposition device, may control operations of relevant components of the atomic layer deposition device, and may implement automatic production of the magnesium fluoride film, which is not specifically limited in this application.
In a third aspect of the embodiments of the present application, a computer-readable storage medium is provided, and fig. 4 is a schematic structural block diagram of the computer-readable storage medium provided in the embodiments of the present application. As shown in fig. 4, the computer-readable storage medium 600 has a computer program 610 stored thereon, and the computer program 610, when executed by a processor, implements the method for preparing a magnesium fluoride thin film according to the first aspect.
The preparation method of the magnesium fluoride film comprises the following steps:
the substrate is transferred to an atomic layer deposition reaction chamber.
And under the condition that the atomic layer deposition reaction chamber reaches the preparation condition, introducing a magnesium source into the atomic layer deposition reaction chamber and then performing gas purging on the atomic layer deposition reaction chamber.
And after the fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber.
The computer program on the computer-readable storage medium provided in the embodiment of the present application may program a method for preparing a magnesium fluoride thin film, where the content of the programming may include an execution time, an order, an execution parameter, and the like of each step, and may implement automation of the method for preparing a magnesium fluoride thin film, and the embodiment of the present application is not particularly limited.
It should be noted that, in the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and reference may be made to relevant descriptions of other embodiments for parts that are not described in detail in a certain embodiment.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as a method, system, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-readable storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and the like) having computer-readable program code embodied therein.
The present application is described with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the application. It will be understood that each flow and/or block of the flow diagrams and/or block diagrams, and combinations of flows and/or blocks in the flow diagrams and/or block diagrams, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, embedded computer, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be stored in a computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner, such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
Embodiments of the present application also provide a computer program product, which includes computer software instructions that, when run on a processing device, cause the processing device to execute the process of the method for preparing a magnesium fluoride thin film.
The computer program product includes one or more computer instructions. The procedures or functions according to the embodiments of the present application are all or partially generated when the computer program instructions are loaded and executed on a computer. The computer may be a general purpose computer, a special purpose computer, a network of computers, or other programmable device. The computer instructions may be stored on a computer readable storage medium or transmitted from one computer readable storage medium to another computer readable storage medium, for example, the computer instructions may be transmitted from one website, computer, server, or data center to another website, computer, server, or data center via wire (e.g., coaxial cable, fiber optic, Digital Subscriber Line (DSL)) or wireless (e.g., infrared, wireless, microwave, etc.). A computer-readable storage medium may be any available medium that a computer can store or a data storage device, such as a server, a data center, etc., that is integrated with one or more available media. The usable medium may be a magnetic medium (e.g., floppy disk, hard disk, magnetic tape), an optical medium (e.g., DVD), or a semiconductor medium (e.g., Solid State Disk (SSD)), among others.
It is clear to those skilled in the art that, for convenience and brevity of description, the specific working processes of the above-described systems, apparatuses and units may refer to the corresponding processes in the foregoing method embodiments, and are not described herein again.
In the several embodiments provided in the present application, it should be understood that the disclosed apparatus, device and method may be implemented in other manners. For example, the above-described apparatus embodiments are merely illustrative, and for example, a division of a unit is merely a logical division, and an actual implementation may have another division, for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed mutual coupling or direct coupling or communication connection may be an indirect coupling or communication connection through some interfaces, devices or units, and may be in an electrical, mechanical or other form.
Units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, functional units in the embodiments of the present application may be integrated into one processing unit, or each unit may exist alone physically, or two or more units are integrated into one unit. The integrated unit can be realized in a form of hardware, and can also be realized in a form of a software functional unit.
The integrated unit, if implemented in the form of a software functional unit and sold or used as a stand-alone product, may be stored in a computer readable storage medium. Based on such understanding, the technical solution of the present application may be substantially implemented or contributed to by the prior art, or all or part of the technical solution may be embodied in a software product, which is stored in a storage medium and includes instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method of the embodiments of the present application. And the aforementioned storage medium includes: various media capable of storing program codes, such as a usb disk, a removable hard disk, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk, or an optical disk.
The above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
While preferred embodiments of the present specification 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 the preferred embodiment and all changes and modifications that fall within the scope of the specification.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present specification without departing from the spirit and scope of the specification. Thus, if such modifications and variations of the present specification fall within the scope of the claims of the present specification and their equivalents, the specification is intended to include such modifications and variations.
Claims (10)
1. A method for preparing a magnesium fluoride film is characterized by comprising the following steps:
transferring the substrate to an atomic layer deposition reaction chamber;
under the condition that the atomic layer deposition reaction chamber meets the preparation condition, a magnesium source is introduced into the atomic layer deposition reaction chamber, and then the atomic layer deposition reaction chamber is subjected to gas purging;
and after a fluorine source is introduced into the atomic layer reaction chamber, performing gas purging on the atomic layer deposition reaction chamber.
2. The method for preparing a magnesium fluoride thin film according to claim 1, further comprising:
and after the fluorine source is introduced into the atomic layer deposition reaction chamber for the set times and the gas purging is completed, controlling the atomic layer deposition reaction chamber to be cooled to the room temperature to obtain the magnesium fluoride film.
3. The method for preparing a magnesium fluoride thin film according to claim 1, wherein the single-pass time of the magnesium source is in a range of 0.001 to 5s, the single-pass time of the fluorine source is in a range of 0.001 to 10s, and the single-pass time of the gas purge is in a range of 1 to 180 s.
4. The method of claim 1, wherein the preparation conditions of the atomic layer deposition reaction chamber include that the substrate is heated to 25-500 ℃ in the atomic layer deposition reaction chamber, a pipe connected to the atomic layer deposition reaction chamber is heated to 25-200 ℃, the temperature of the atomic layer deposition reaction chamber is 25-200 ℃, and the temperature of the magnesium source and the fluorine source is 25-200 ℃.
5. The method for producing a magnesium fluoride thin film according to claim 4, wherein the substrate comprises silicon, sapphire, or glass;
the magnesium source comprises at least one of magnesium neodecanoate, magnesium 2,2,6, 6-tetramethyl-3, 5-heptanedionate, magnesium trifluoroacetylacetonate, magnesium hexafluoroacetylacetonate, magnesium acetylacetonate, magnesium metallocenes and bis-ethylcyclopentadienyl magnesium;
the fluorine source includes at least one of elemental fluorine and hydrogen fluoride.
6. The method of claim 5, wherein in the case where the substrate is sapphire, the magnesium source is bis-ethylcyclopentadienyl magnesium, and the fluorine source is hydrogen fluoride, the preparation conditions of the atomic layer deposition reaction chamber are as follows:
the substrate is heated to 100 ℃, the temperature of the atomic layer deposition reaction chamber is 100 ℃, a pipeline connected with the atomic layer deposition reaction chamber is heated to 100 ℃, the temperature range of the magnesium source is 60-100 ℃, and the temperature of the fluorine source is 25 ℃.
7. The method for preparing a magnesium fluoride thin film according to claim 5, wherein in the case where the magnesium source is bis-ethylcyclopentadienyl magnesium and the fluorine source is hydrogen fluoride, the introduction time of the magnesium source is in the range of 0.5 to 1.2s, the introduction time of the fluorine source is in the range of 2 to 8s, and the gas purge time is in the range of 20 to 60 s.
8. The method for preparing a magnesium fluoride thin film according to claim 1, wherein the gas used for the gas purge includes at least one of an inert gas and nitrogen.
9. An electronic device, comprising:
a memory having a computer program stored therein;
a processor for implementing the method of preparing a magnesium fluoride thin film according to any one of claims 1 to 8 when executing the computer program.
10. A computer-readable storage medium, wherein a computer program is stored thereon, and when executed by a processor, the computer program implements the method for preparing a magnesium fluoride thin film according to any one of claims 1 to 8.
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