CN111101204A - Single crystal AlN film and preparation method and application thereof - Google Patents
Single crystal AlN film and preparation method and application thereof Download PDFInfo
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- CN111101204A CN111101204A CN201911275256.2A CN201911275256A CN111101204A CN 111101204 A CN111101204 A CN 111101204A CN 201911275256 A CN201911275256 A CN 201911275256A CN 111101204 A CN111101204 A CN 111101204A
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- 239000013078 crystal Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 48
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 48
- 239000010408 film Substances 0.000 claims abstract description 45
- 239000010409 thin film Substances 0.000 claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 39
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- 239000003990 capacitor Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000013077 target material Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000003989 dielectric material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000011161 development Methods 0.000 abstract description 6
- 238000000151 deposition Methods 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 238000004549 pulsed laser deposition Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 3
- 150000002902 organometallic compounds Chemical class 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
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- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 1
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- 238000004020 luminiscence type Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 230000003000 nontoxic effect Effects 0.000 description 1
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- 230000005855 radiation 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
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 238000007736 thin film deposition technique Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
Abstract
The invention belongs to the technical field of film preparation and discloses single crystal Al2O3A preparation method and application of a/TiN/AlN film; the single crystal Al is prepared by a pulse laser deposition method by controlling the growth temperature of the AlN film, selecting the energy flow density of the AlN film, the energy flow density of the TiN bottom electrode and controlling the nitrogen pressure in the cavity2O3The method has simple preparation process, simple and convenient operation and easy realization, and the prepared single crystal Al is2O3the/TiN/AlN thin film has good ductility and crystallinity, excellent compactness and flatness, excellent dielectric property when used in a dielectric capacitor for radio frequency front end operation, and high capacitanceThe device has non-adjustability and great development and application values.
Description
Technical Field
The invention relates to the technical field of single crystal film preparation, in particular to a single crystal AlN film and a preparation method and application thereof.
Background
Dielectric materials are a special electrical property of partial insulating materials, and with the development of miniaturization and high performance of electronic devices, the dielectric materials are receiving great attention from researchers. The dielectric energy storage technology has the characteristics of extremely high energy conversion rate, long working time, environmental friendliness and the like, and is originally exposed in the fields of modern electronic and power industries such as wearable electronic equipment, hybrid electric vehicles, weapon systems and the like. With the development of electronic devices toward miniaturization and high performance, a dielectric material having a high energy storage density is in urgent need.
With the high-speed development of the fifth generation mobile communication, key indexes such as end-to-end time delay, connection end density, peak rate, user downloading rate and mobility are greatly improved compared with the previous generations. The abundance of mobile communication technology and the application of emerging internet of things have further requirements on 5G devices and modules, including long battery life, high reliability and the like. This places more stringent requirements on the loss characteristics, power capability, operating frequency and high integration of the rf front-end device.
The III-V group nitride semiconductor material comprises aluminum nitride, gallium nitride, indium nitride and alloy thereof, and has the characteristics of large forbidden bandwidth, high electronic saturation velocity, small dielectric constant, good heat-conducting property and the like, so the III-V group nitride semiconductor material has unique advantages in the aspects of radiation-resistant, high-frequency and high-power electronic devices, luminescent devices and photodetectors. The AlN material has the advantages of ultraviolet short-wave luminescence at room temperature, good surface acoustic wave resonance and the like, is nontoxic and stable in chemical property, becomes an excellent material for preparing photoelectron and microelectronic devices and has great development and application values.
Pulsed laser deposition is a vacuum thin film deposition technique which bombards a ceramic or single crystal target with high-energy pulsed laser and deposits the target material on a corresponding substrate to form a film. Pulse laser deposition technology is one of important film-making technologies, has gained the attention of researchers, and is applied to the preparation of various thin films of oxides, nitrides, sulfides, and the like, and multilayer films.
At present, the preparation method for growing the AlN film by heteroepitaxy develops more and more mature, and mainly comprises a reaction magnetron sputtering method, a chemical vapor deposition method, molecular beam epitaxy, metal organic compound vapor deposition, hydride vapor phase epitaxy and the like. The magnetron sputtering method adopts radio frequency bombardment target materials, the growth speed is high, but the grown film is basically polycrystalline. Too fast a growth rate is only suitable for growing thick film materials. Metal organic compound vapor deposition is a method commonly used today for growing nitride thin films. It is suitable for large area growing film and has fast growth speed. However, it is difficult to grow AlN material and AlGaN having high Al composition, because when a thin film is grown under low pressure, a trimethylaluminum source is strongly irreversibly pre-reacted with ammonia, and AlN atoms are difficult to incorporate into a crystal lattice, resulting in a decrease in growth rate and a decrease in material crystal quality. Meanwhile, the vapor deposition of metal organic compounds requires high running cost and uses toxic metal organic sources. The molecular beam epitaxy adopts crucible heating and vacuum evaporation, and can realize the precise control of the growth of quantum wells and superlattice structures. It needs to be carried out in a high vacuum environment, the air pressure is usually above in the growth process, and pre-reaction hardly exists. However, the molecular beam epitaxy is performed by heating and vacuum evaporation in a crucible, which generally causes crucible pollution; meanwhile, the Al furnace is easy to crack, energy needs to be consumed to maintain the temperature of the Al furnace above the melting point of Al metal, otherwise the Al furnace is easy to scrap, and the operation cost is high. And the two methods are easy to generate interface reaction.
Meanwhile, in the conventional research, the AlN thin film was studied only as a sacrificial layer for growing GaN, and it was rarely prepared and studied as a dielectric capacitor alone.
Disclosure of Invention
In view of the above problems in the prior art, it is a primary object of the present invention to provide a single crystal Al2O3A preparation method of a TiN/AlN film.
The second purpose of the invention is to provide the single crystal Al prepared by the method2O3a/TiN/AlN thin film.
It is a third object of the present invention to provide a composition comprising single-crystal Al2O3A dielectric material of/TiN/AlN thin film.
It is a fourth object of the present invention to provide single-crystal Al2O3The application of the/TiN/AlN film in the preparation of a dielectric capacitor.
The purpose of the invention is realized by the following technical scheme:
single crystal Al2O3The preparation method of the/TiN/AlN film comprises the following steps:
s1, cleaning Al2O3A substrate;
s2, heating Al2O3Substrate, selecting energy flow density suitable for TiN bottom electrode, in Al2O3Growing a TiN bottom electrode on the substrate;
s3, heating Al2O3Substrate of Al2O3The substrate temperature reaches the temperature range suitable for the growth of the AlN thin film;
s4, vacuumizing to enable the vacuum degree in the cavity to reach 10-4Pa, then introducing high-purity nitrogen to ensure that the nitrogen pressure in the cavity reaches 5 multiplied by 10-4Pa～1×10-3Pa, selecting energy flow density suitable for AlN film growth to grow AlN film on TiN bottom electrode, cooling to room temperature to obtain monocrystal Al2O3a/TiN/AlN thin film;
the energy flow density of the AlN thin film is at least 4 times higher than that of the TiN bottom electrode; the temperature range suitable for the growth of the AlN thin film in the step S3 is 700-800 ℃.
Experiments show that only in the process of pulse laser deposition, the growth temperature of the AlN film is controlled, the energy flow density of the AlN film is selected, the energy flow density of the TiN bottom electrode is selected, and the nitrogen pressure in the cavity is controlled; can ensure that single crystal Al is obtained2O3a/TiN/AlN thin film.
In the invention, when the AlN thin film is prepared by using a pulse laser deposition method, a TiN bottom electrode is used, because the bottom electrode is needed in consideration of the AlN thin film used in a dielectric container, and of course, other bottom electrodes commonly used in the dielectric container, such as zirconium nitride, can be selected and used; when other bottom electrodes such as zirconium nitride are used, other process conditions in pulsed laser deposition need to be additionally adjusted, so that the AlN thin film with the composite requirement is obtained.
In some specific embodiments, the distance between the TiN bottom electrode and the target material is 4-4.5 cm; the flatness of the finally obtained film can be influenced by the distance between the target and the substrate, and the flatness of the prepared film is the best when the distance between the TiN bottom electrode and the target is 4-4.5 cm.
In some embodiments, the Al is cleaned in step S12O3The substrate is specifically operative to: cleaning Al with acetone, isopropanol and alcohol respectively2O3Drying the substrate by nitrogen; the three organic solvents are adopted to clean the surface of the substrate, so that the flatness of the surface of the substrate is better, and a film with good flatness is facilitated.
In some embodiments, step S3 heats the substrate with a temperature ramp at a rate of 5-10 ℃/min, which helps to protect the substrate from cracks due to sudden temperature increases. Affecting the properties and quality of the final film.
In some embodiments, step S4 employs gradual cooling to room temperature at a cooling rate of 2-5 ℃/min, which helps stabilize the quality of the film.
The invention also provides a dielectric material, which comprises the monocrystalline Al prepared by the method2O3a/TiN/AlN thin film.
The invention also provides the single crystal Al prepared by the method2O3The application of the/TiN/AlN film in the preparation of a dielectric capacitor.
In particular, the dielectric container is made of single crystal Al2O3the/TiN/AlN film is made of metal; the dielectric capacitor is used for preparing dielectric layers of radio frequency front-end devices and integrated circuit wiring, and replaces SiO2An insulating layer of an SOI structure, etc.
Compared with the prior art, the invention has the beneficial effects that:
the single crystal Al is prepared by a pulse laser deposition method by controlling the growth temperature of the AlN film, selecting the energy flow density of the AlN film, the energy flow density of the TiN bottom electrode and controlling the nitrogen pressure in the cavity2O3The method has simple preparation process, simple and convenient operation and easy realization, and the prepared single crystal Al is2O3the/TiN/AlN thin film has good ductility and crystallinity, and also has excellent compactness and flatness, when the dielectric thin film is used for a dielectric capacitor working at a radio frequency front end, the dielectric property is excellent, and the capacitor has non-adjustability and great development and application values.
Drawings
FIG. 1 shows single crystal Al2O3X-ray diffraction peak of/TiN/AlN thin film;
FIG. 2 shows single crystal Al2O3the/TiN/AlN film atomic force microscope appearance picture;
FIG. 3 is Al2O3C-F (capacitance change with frequency) diagram of/TiN/AlN/Ni + Au capacitor;
FIG. 4 shows Al2O3C-V (capacitance change with voltage) diagram of/TiN/AlN/Ni + Au capacitor;
FIG. 5 shows Al2O3The structure of the/TiN/AlN/Ni + Au capacitor is shown schematically.
Detailed Description
For a more clear understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Single crystal Al2O3The preparation method of the/TiN/AlN film comprises the following steps:
(1) firstly, to single crystal Al2O3SubstrateTreating, and cleaning single crystal Al with acetone, isopropanol, and alcohol respectively2O3The substrate is finally blown dry by nitrogen gas, so that the single crystal Al2O3The surface of the substrate is free from pollution.
(2) The energy in the cavity is represented by an energy meter, and energy flow densities suitable for the growth of the AlN thin film and the TiN bottom electrode are respectively selected, wherein in the embodiment, the energy flow density for the growth of the AlN thin film is 8.75J/cm2The energy flow density of TiN bottom electrode growth is 2J/cm2The laser frequency was set at 5 Hz.
(3) Using silver glue to make monocrystal Al2O3The substrate is attached to a heating table, the heating rate is set to be 5 ℃/min, and the temperature of the single crystal Al is controlled2O3Growing TiN bottom electrode on the substrate, wherein the target material is TiN ceramic target material, and the vacuum degree is 7 multiplied by 10-4Pa, laser fluence of 2J/cm2。
(4) Heating Al2O3Substrate of Al2O3The substrate temperature reached 700 deg.c.
(5) Pumping the chamber to a vacuum degree of 10 in the chamber of the pulsed laser deposition system-4Pa, so that the nitrogen content of the cavity reaches 10-4Pa; then high-purity nitrogen is introduced to ensure that the pressure of the nitrogen in the cavity reaches 5 multiplied by 10-4Pa。
(6) Selecting a high-purity AlN ceramic target as a precursor, adjusting the distance between the TiN bottom electrode and the target to be 4cm, bombarding the surface of the AlN ceramic target by using selected laser energy, and growing an AlN thin film on the TiN bottom electrode.
(7) Cooling, cooling to room temperature at the speed of 2 ℃/min to obtain the single crystal Al2O3a/TiN/AlN thin film.
Example 2
Single crystal Al2O3The preparation method of the/TiN/AlN film comprises the following steps:
(1) firstly, to single crystal Al2O3Treating the substrate, and respectively cleaning the single crystal Al with acetone, isopropyl alcohol and alcohol2O3The substrate is finally blown dry by nitrogen gas, so that the single crystal Al2O3Substrate surfaceNo pollution.
(2) The energy in the cavity is represented by an energy meter, and energy flow densities suitable for the growth of the AlN thin film and the TiN bottom electrode are respectively selected, wherein in the embodiment, the energy flow density for the growth of the AlN thin film is 9J/cm2The energy flow density of TiN bottom electrode growth is 2.2J/cm2The laser frequency was set at 5 Hz.
(3) Using silver glue to make monocrystal Al2O3The substrate is attached to a heating table, the heating rate is set to be 8 ℃/min, and the temperature of the single crystal Al is controlled2O3Growing TiN bottom electrode on the substrate, wherein the target material is TiN ceramic target material, and the vacuum degree is 7 multiplied by 10-4Pa, laser fluence of 2.2J/cm2。
(4) Heating Al2O3Substrate of Al2O3The substrate temperature reached 750 ℃.
(5) Pumping the chamber to a vacuum degree of 10 in the chamber of the pulsed laser deposition system-4Pa, so that the nitrogen content of the cavity reaches 10-4Pa; then high-purity nitrogen is used to make the nitrogen pressure in the cavity reach 8 x 10-4Pa。
(6) Selecting a high-purity AlN ceramic target as a precursor, adjusting the distance between the TiN bottom electrode and the target to be 4.25cm, bombarding the surface of the AlN ceramic target by using selected laser energy, and growing an AlN thin film on the TiN bottom electrode.
(7) Cooling, cooling to room temperature at a rate of 3.5 ℃/min to obtain the single crystal Al2O3a/TiN/AlN thin film.
Example 3
Single crystal Al2O3The preparation method of the/TiN/AlN film comprises the following steps:
(1) firstly, to single crystal Al2O3Treating the substrate, and respectively cleaning the single crystal Al with acetone, isopropyl alcohol and alcohol2O3The substrate is finally blown dry by nitrogen gas, so that the single crystal Al2O3The surface of the substrate is free from pollution.
(2) The energy inside the cavity was characterized by an energy meter, and the energy flux densities suitable for the growth of AlN thin film and TiN bottom electrode were selected respectively, in this exampleThe energy flow density of the AlN thin film growth is 8.5J/cm2The energy flow density of TiN bottom electrode growth is 2.1J/cm2The laser frequency was set at 5 Hz.
(3) Using silver glue to make monocrystal Al2O3The substrate is attached to a heating table, the heating rate is set to be 10 ℃/min, and the temperature of the single crystal Al is controlled2O3Growing TiN bottom electrode on the substrate, wherein the target material is TiN ceramic target material, and the vacuum degree is 10-4，。
(4) Heating Al2O3Substrate of Al2O3The substrate temperature reached 800 ℃.
(5) Pumping the chamber to a vacuum degree of 10 in the chamber of the pulsed laser deposition system-4Pa, so that the nitrogen content of the cavity reaches 10-4Pa; then high-purity nitrogen is used to make the nitrogen pressure in the cavity reach 1 x 10-3Pa。
(6) Selecting a high-purity AlN ceramic target as a precursor, adjusting the distance between the TiN bottom electrode and the target to be 4.5cm, bombarding the surface of the AlN ceramic target by using selected laser energy, and growing an AlN thin film on the TiN bottom electrode.
(7) Cooling, cooling to room temperature at the speed of 5 ℃/min to obtain the single crystal Al2O3a/TiN/AlN thin film.
For the single crystal Al prepared in example 32O3the/TiN/AlN thin film is characterized, and the results are shown in figure 1, figure 2 and figure 12O3X-ray diffraction peak chart of/TiN/AlN thin film shows single crystal Al prepared2O3the/TiN/AlN film has a good crystal structure and is a hexagonal aluminum nitride film and a hexagonal titanium nitride film. FIG. 2 shows single crystal Al2O3The result of the atomic force microscope morphology picture of the/TiN/AlN film shows that the prepared single crystal Al2O3the/TiN/AlN thin film has good crystallinity and very good surface flatness.
Single crystal Al produced in example 32O3Preparation of Al by/TiN/AlN film assembly2O3The dielectric properties of the/TiN/AlN/Ni + Au capacitor were examined, and the results are shown in FIG. 3 and FIG. 4, in which FIG. 3 is that of the capacitorA plot of relative dielectric constant versus frequency shows that the dielectric constant of the thin film capacitor is 2 times greater than reported, 18. FIG. 4 is a graph of the relative dielectric constant of a capacitor as a function of voltage showing that the dielectric constant of a thin film capacitor is 2 times greater than reported, 18. Also, it is shown that the dielectric constant of the film is not tunable. The single crystal Al advantageously prepared by the present invention is illustrated by the above two figures2O3The capacitor assembled by the/TiN/AlN film has good dielectric property, and meanwhile, the capacitance is known to have non-adjustability.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. Single crystal Al2O3The preparation method of the/TiN/AlN thin film is characterized by comprising the following steps of:
s1, cleaning Al2O3A substrate;
s2, heating Al2O3Substrate, selecting energy flow density suitable for TiN bottom electrode, in Al2O3Growing a TiN bottom electrode on the substrate;
s3, heating Al2O3Substrate of Al2O3The substrate temperature reaches the temperature range suitable for the growth of the AlN thin film;
s4, vacuumizing to enable the vacuum degree in the cavity to reach 10-4Pa, then introducing high-purity nitrogen to ensure that the nitrogen pressure in the cavity reaches 5 multiplied by 10-4Pa～1×10-3Pa, selecting energy flow density suitable for AlN film growth to grow AlN film on TiN bottom electrode, cooling to room temperature to obtain monocrystal Al2O3a/TiN/AlN thin film;
the energy flow density of the AlN thin film is at least 4 times higher than that of the TiN bottom electrode; the temperature range suitable for the growth of the AlN thin film in the step S3 is 700-800 ℃.
2. The single-crystal Al according to claim 12O3The preparation method of the/TiN/AlN thin film is characterized in that the distance between the TiN bottom electrode and the target material is 4-4.5 cm.
3. The single-crystal Al according to claim 12O3The preparation method of the/TiN/AlN thin film is characterized in that the Al is cleaned in the step S12O3The substrate is specifically operative to: cleaning Al with acetone, isopropanol and alcohol respectively2O3The substrate is finally blown dry with nitrogen.
4. The single-crystal Al according to claim 12O3The preparation method of the/TiN/AlN film is characterized in that the substrate is heated by gradually raising the temperature in the step S3, wherein the temperature raising rate is 5-10 ℃/min.
5. The single-crystal Al according to claim 12O3The preparation method of the/TiN/AlN film is characterized in that step S4 adopts gradual cooling to room temperature, and the cooling rate is 2-5 ℃/min.
6. A dielectric material comprising single-crystal Al prepared by the method of any one of claims 1 to 52O3a/TiN/AlN thin film.
7. Single crystal Al produced by the method of any one of claims 1 to 52O3The application of the/TiN/AlN film in the preparation of a dielectric capacitor.
8. Use according to claim 7, wherein the dielectric container is made of single-crystal Al2O3a/TiN/AlN thin film and a metal.
9. The method of claim 8The dielectric container is used for preparing dielectric layers of radio frequency front-end devices and integrated circuit wiring, and SiO is replaced2And (5) making an insulating layer of an SOI structure.
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| CN111962153A (en) * | 2020-07-03 | 2020-11-20 | 华南师范大学 | Single crystal TiN electrode film and preparation method thereof |
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