CN110158048A - The method and its application of ultra-thin high quality oxide film are grown on two-dimensional layer material - Google Patents
The method and its application of ultra-thin high quality oxide film are grown on two-dimensional layer material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000010410 layer Substances 0.000 claims abstract description 101
- 239000002356 single layer Substances 0.000 claims abstract description 38
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 21
- 238000000407 epitaxy Methods 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 73
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 62
- 229910021389 graphene Inorganic materials 0.000 claims description 61
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 241000588731 Hafnia Species 0.000 claims description 13
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 230000005669 field effect Effects 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 5
- 238000006263 metalation reaction Methods 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical compound N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000071 diazene Inorganic materials 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims 2
- 229910052582 BN Inorganic materials 0.000 claims 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000003949 imides Chemical class 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 2
- 239000010453 quartz Substances 0.000 description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 40
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 25
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 20
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 20
- 238000000089 atomic force micrograph Methods 0.000 description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 18
- 229910052710 silicon Inorganic materials 0.000 description 18
- 239000010703 silicon Substances 0.000 description 18
- 239000002120 nanofilm Substances 0.000 description 16
- 239000003708 ampul Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000012546 transfer Methods 0.000 description 12
- 238000000151 deposition Methods 0.000 description 11
- 238000010792 warming Methods 0.000 description 11
- 230000008021 deposition Effects 0.000 description 10
- 230000015556 catabolic process Effects 0.000 description 9
- 229910000449 hafnium oxide Inorganic materials 0.000 description 9
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 6
- 230000036760 body temperature Effects 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- -1 Phenyl acid imide Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 230000005641 tunneling Effects 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- 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
- C23C16/40—Oxides
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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]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/28008—Making conductor-insulator-semiconductor electrodes
- H01L21/28017—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon
- H01L21/28158—Making the insulator
- H01L21/28167—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation
- H01L21/28194—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation by deposition, e.g. evaporation, ALD, CVD, sputtering, laser deposition
Abstract
The present invention discloses a kind of method and its application that ultra-thin high quality oxide film is grown on two-dimensional layer material, and this method comprises the following steps: (1) single layer organic dye molecule film is grown on two-dimensional layer material using Van der Waals epitaxy growing technology；(2) sull of ultra-thin homogeneous is grown on two-dimensional layer material using single layer organic dye molecule film as seed layer using technique for atomic layer deposition.The present invention does seed layer in the organic dye molecule film that two-dimensional layer material surface grows single layer by Van der Waals epitaxy, it can accomplish almost not damaged to two-dimensional layer material, and can deposit to obtain ultra-thin and even compact high quality oxide film in the seed layer；Meanwhile the growing method is low in cost, processing is realized simple；Using sull prepared by the method for the present invention excellent uniformity and resistance to pressure, the electronic device applications being applicable under diversified forms can be still kept in the case where very thin.
Description
Technical field
The present invention relates to a kind of to grow the method for ultra-thin high quality oxide film and its is used on two-dimensional layer material
The application for preparing electronic device belongs to two-dimensional material field of electronic devices.
Background technique
In recent decades, under the guidance of Moore's Law, characteristic size constantly reduces silicon-based electronic devices.But with ruler
Degree gradually approaches quantum limit, limits further reducing for silicon-based electronic devices size including the problems such as short-channel effect.It grinds
Studying carefully with Development of Novel material is one of the main path for continuing Moore's Law.Since graphene is found, more and more
Two-dimensional layer material due to its power, heat, light, in terms of excellent properties, receive the concern of people.In two-dimensional material face
Generally by covalent bonding, and interlayer is only combined by Van der Waals for, this characteristic, which allows us to obtain, has original
The single layer two-dimensional material of sub- grade, thickness is generally at 1 nanometer or less.Due to the atomic-level thickness of two-dimensional material, so as to
The preparation that nanometer grid length device of excellent performance, especially 1 is still kept in short channel device presents silicon-based electronic devices institute
The advantage not having.
Currently, the oxide that a significant challenge of limitation two-dimensional layer material logical device development is depositing high-quality is situated between
Electric layer.Since two-dimensional layer material surface is without dangling bonds, atomic layer deposition sull is directly utilized on it, there are coarse
Degree is big, has the problems such as stomata, discontinuous, not fine and close, uneven, it is suppressed that the development of two-dimensional layer material top-gated device and answers
With.Currently used method is the deposited metal in two-dimensional material, and seed layer is used as after oxidation.It is high but when deposited metal
The metallic vapour energy of temperature is larger, is easy to damage two-dimensional material, generates many defects, moreover, when deposited metal is as seed layer,
In order to guarantee the abundant covering to two-dimensional material, required metal thickness is thicker, cannot achieve ultrathin oxide deposition.Its other party
Method is functionalized two-dimensional material surface using gases such as plasma, ozone etc., increases two-dimensional material surface hydrophilicity, into
And deposition oxide dielectric layer, but some irreversible damages can be generated to two-dimensional material.The method of open report is equal at present
It is difficult to obtain uniform ultra-thin high quality oxide film.
Based on this, inventor develops one kind epitaxial growth single layer two dimension organic molecular film in two-dimensional material and is used as kind
Sublayer, and then grow the method for high-quality ultra-thin even oxide.
Summary of the invention
Goal of the invention: it is damaged existing for the method for growing oxide film in two-dimensional material in the prior art two-dimentional
The problems such as material, sull are uneven, discontinuous, not fine and close, the present invention provide one kind and grow on two-dimensional layer material
The method of ultra-thin high quality oxide film, and a kind of application that this method is used to prepare to electronic device is provided.
Technical solution: the method for the present invention that ultra-thin high quality oxide film is grown on two-dimensional layer material,
Include the following steps:
(1) using Van der Waals epitaxy growing technology, that single layer organic dye molecule is grown on two-dimensional layer material is thin
Film；
(2) technique for atomic layer deposition is utilized, using single layer organic dye molecule film as seed layer, in two-dimensional layer material
On grow the sull of ultra-thin homogeneous.
Wherein, two-dimensional layer material includes but is not limited to the Transition-metal dichalcogenides such as graphene and molybdenum disulfide.
Organic dye molecule film includes but is not limited to the film of any formation in following organic dye molecule: 3,4,9,10- tetra-
Acid dianhydride and its derivative, 3,4,9,10- 4 formyl-2-imides and its derivative, rubrene and its derivative, N, N- diformazan
Phenyl acid imide and its derivative.Sull is the sull arbitrarily grown using technique for atomic layer deposition,
Including but not limited to aluminum oxide film, hafnia film, zirconia film, thin film of titanium oxide, oxidation lanthanum film.
It preferably, is growth source by substrate, organic dye molecule of two-dimensional layer material, spacing distance is set in step (1)
In tube furnace, after tubular type stove evacuation, heating furnace body to growth source position at temperature be 240~260 DEG C, heat preservation 0.2~
0.8h evaporates organic dye molecule, and the organic dye molecule film to form single layer is deposited in two-dimensional layer material upper surface.Its
In, 2~4cm placement preferably spaced apart between substrate and growth source.Before starting tube furnace, first tube furnace can be evacuated to very with vacuum pump
It is empty；After starting tube furnace, preferably furnace body first can be warming up to 220~240 DEG C in 10min, then continue to heat up in 5min
To 240~260 DEG C, 0.2~0.8h of heat preservation；After heating, tube furnace is naturally cooling to room temperature, terminates growth.
Preferably, in step (2), the two-dimensional layer material of single layer organic dye molecule film is transferred to atom growth
In layer deposition chamber, vacuumizes, cavity temperature is increased to 80~90 DEG C, source metal and oxidation source are then passed to, in two-dimensional layer
The seed layer surface in situ of shape material deposits to obtain the sull of ultra-thin homogeneous；Lower temperature can guarantee that single layer is organic
Integrality of the dye molecule film on two-dimensional layer material, to guarantee that sull may be implemented in two-dimensional layer material
The deposition of upper ultra-thin homogeneous.Cavity temperature is preferably first increased to 70~80 DEG C, after waiting 5-10min, then by cavity temperature liter
Up to 80~90 DEG C；By this heating mode can guarantee cavity temperature slowly rise, to prevent occur temperature more than target temperature,
The case where influencing sull deposition quality.
The sull of the above-mentioned method preparation that ultra-thin high quality oxide film is grown on two-dimensional layer material can
In the case where very thin, still to keep excellent uniformity and resistance to pressure, it can be used for preparing a variety of electronic devices, such as field-effect
Transistor, tunneling transistor, memory device etc..By taking field effect transistor as an example, preparation method may include following steps:
(1) using Van der Waals epitaxy growing technology, that single layer organic dye molecule is grown on two-dimensional layer material is thin
Film；
(2) technique for atomic layer deposition is utilized, using the single layer organic dye molecule film as seed layer, in two-dimensional layer
Ultra-thin homogeneous sull is grown on material, as dielectric layer；
(3) top-gated electrode is prepared on the two-dimensional layer material for grown ultrathin oxide film, obtains two-dimensional layer material
Stock ground field effect transistor devices.The device includes: two-dimensional layer material from bottom to top, single layer organic dye molecule film, ultra-thin
Sull and metal roof gate electrode.
When preparing FET device, the original of two-dimensional layer material, organic dye molecule film and sull
Expect that range of choice and step (1)~(2) process control procedure grow ultra-thin high quality with above-mentioned on two-dimensional layer material
It is identical in the method for sull.
The utility model has the advantages that compared with the prior art, the advantages of the present invention are as follows: (1) make seed layer with traditional evaporation metal
And the methods of two-dimensional layer material surface functionalization is compared, the present invention is by Van der Waals epitaxy in two-dimensional layer material table
The organic dye molecule film of long single layer of looking unfamiliar does seed layer, can accomplish, Er Qiejie almost not damaged to two-dimensional layer material
It closes the technology controlling and process of atomic layer deposition process, can deposit to obtain ultra-thin and even compact sull in the seed layer；
Meanwhile growing method of the invention is low in cost, processing is realized simple；(2) compared with traditional evaporation metal is as seed layer,
The present invention is only 0.3 nanometer as the thickness of the single layer organic dye molecule film of seed layer, is far below evaporation metal thickness, right
The capacitive effect of whole gate medium is greatly lowered；It (3) can be very thin using the sull of the method for the present invention preparation
In the case of, still keep excellent uniformity and resistance to pressure, the electronic device applications being applicable under diversified forms, including field-effect
Transistor, tunneling transistor, memory device etc. such as can effectively reduce electric leakage using the FET device of this method preparation
Amount alleviates short-channel effect.
Detailed description of the invention
Fig. 1 is the atomic force microscope images of graphene before and after growth seed layer in embodiment 1, wherein (a) is to be transferred
Atomic force microscope images on to silicon wafer as the graphene of substrate (b) are that grown 3,4,9,10- tetracid dianhydride of single layer
The atomic force microscope images of the graphene of molecular film；
Fig. 2 is the atomic force microscope images that graphene after hafnia film is grown using distinct methods, wherein (a) is
The atomic force microscope images of the graphene of hafnia film growth are completed in embodiment 1, (b) are direct on graphene substrate
Grow the atomic force microscope images of hafnia film；
Fig. 3 is the scanning electron microscope (SEM) photograph that the double grid graphene prepared after hafnia film growth is completed in embodiment 1；
Fig. 4 a is the transfer characteristic curve that the graphene device scans top-gated voltage under different back gate voltages, and Fig. 4 b is pair
To extract the top-gated voltage-back gate voltage variation drawn bent for graphene dirac point under different top gate voltage and backgate top-gated in Fig. 4 a
Line；
Fig. 5 a is the breakdown indicatrix of the graphene double-gated devices of different hafnium oxide thickness；Fig. 5 b is to have counted different oxygen
Change the breakdown voltage and breakdown electric field of 30 graphene double-gated devices of hafnium thickness；Fig. 5 c is that 30 graphene double-gated devices are being pushed up
Gate voltage is equal to gate leak current surface density at 1 volt；
Fig. 6 is the atomic force microscope images that the graphene of zirconia film growth is completed in embodiment 2；
Fig. 7 is the atomic force microscope images that the graphene of aluminum oxide film growth is completed in embodiment 3；
Fig. 8 is to make seed layer using 3,4,9,10- 4 formyl-2-imide molecular film of single layer in embodiment 4, in graphite
The atomic force microscope images of aluminum oxide film growth are completed on alkene；
Fig. 9 is the atomic force microscope images of graphene before and after growth seed layer in embodiment 5, wherein (a) is to be transferred
Atomic force microscope images on to silicon wafer as the molybdenum disulfide of substrate (b) are that grown 3,4,9,10- tetracid two of single layer
The atomic force microscope images of the molybdenum disulfide of acid anhydride molecular film；
Figure 10 is the atomic force microscope images that the molybdenum disulfide of hafnium oxide growth is completed in embodiment 5；
Figure 11 a is the transfer that the molybdenum disulfide device prepared in embodiment 5 scans top-gated voltage under different back gate voltages
Characteristic curve, Figure 11 b are to extract the top-gated drawn to graphene dirac point under different top gate voltage in Figure 11 a and back gate voltage
Voltage-back gate voltage change curve.
Specific embodiment
Technical solution of the present invention is described further with reference to the accompanying drawing.
The method that ultra-thin high quality oxide film is grown on two-dimensional layer material of the invention, using in two-dimensional layer
The single layer organic dye molecule film of material surface Van der Waals epitaxy passes through atomic layer deposition two as seed layer
The sull of ultra-thin high quality is prepared on dimension stratified material.Which ensure that the electronic device based on two-dimensional layer material
The preparation of (such as FET device), for two-dimensional layer material, in logic/analog circuit, further application has been created
Sharp condition.
Embodiment 1
1) graphene two-dimensional layer material is prepared using mechanical stripping method, and graphene two-dimensional layer material is transferred to silicon
On piece, and upper source-drain electrode is prepared in the two sides of graphene；Such as Fig. 1 (a), it is transferred to the thin graphene on silicon wafer as substrate
With a thickness of 1.1nm.
2) 3,4,9,10- tetracid dianhydride powder are put into quartz boat, as growth source, and quartz boat are put into tubular type
Furnace center；Silicon wafer that transfer has graphene is placed on another quartz boat, and this quartz boat is put into quartz ampoule, and is held
The quartz boat of 3,4,9,10- tetracid dianhydride powder is at a distance of 2 centimetres；After placement, quartz ampoule is installed corresponding to tube furnace
Position, and vacuumize；
3) tube furnace is started, is warming up to 240 DEG C within furnace body temperature 10 minutes, then 260 DEG C is warming up within 5 minutes, at 260 DEG C
It maintains 0.2 hour, 3,4,9,10- tetracid dianhydride powder grow source evaporation, and deposit on graphene；It, will after heating
Tube furnace is naturally cooling to room temperature, terminates growth.
4) graphene of single layer 3,4,9,10- tetracid dianhydride molecular film moves to atomic layer from quartz ampoule growth
In deposition chamber, vacuum pumping is carried out to atomic layer deposition cavity, and cavity temperature is increased to 80 DEG C, wait 10min
Afterwards, then by cavity temperature 90 DEG C are increased to；
5) after cavity/cavity wall temperature reaches rated temperature, using four (dimethylamino) hafniums as the metal of atomic layer deposition
Source, water set cycle-index as oxidation source, and source metal and oxidation source each burst length are respectively 250ms and 60ms,
Scavenging period between two subpulses is 60s；The hafnia film of 1.5nm thickness is grown on the surface of graphene.
Fig. 1 (b) makes a living the atomic force of the thin graphene sample with single layer 3,4,9,10- tetracid dianhydride molecular film
MIcrosope image, substrate surface graphene and monomolecular film with a thickness of 1.4nm, compared with Fig. 1 (a), it can be found that thick
Degree increases 0.3nm, exactly single layer 3, the thickness of 4,9,10- tetracid dianhydride molecular films；Moreover, can from its surface topography
To find out, 3,4,9,10- tetracid dianhydride molecular film of single layer may be implemented uniformly to arrange on graphene.
Fig. 2 (a) is the atomic force microscope images for having grown hafnium oxide, and Fig. 2 (b) is directly to grow on graphene substrate
The atomic force microscope images of hafnia film, the two comparison show to make seed layer in two dimension using single layer two-dimensional molecular film
The method of ultra-thin high quality oxide film is grown on stratified material, can prepare the oxidation of uniform ground on the surface of graphene
Hafnium film.
6) top-gated electrode is prepared in the graphene sample for grown hafnia film, and double grid test is carried out to device.
Fig. 3 is the scanning electron microscope image of the thin graphene double-gated devices of preparation.
Fig. 4 a is the transfer characteristic curve that the graphene device scans top-gated voltage under different back gate voltages.Fig. 4 b is benefit
With the transfer characteristic curve of Fig. 4 a, top-gated voltage-back gate voltage curve that graphene dirac point-rendering goes out is extracted, it therefrom can be with
Top-gated capacitor is obtained to the ratio of backgate capacitor, top-gated capacitivity: backgate capacitivity=183, since backgate is 275nm oxidation
Silicon, then the equivalent oxide thickness of the hafnia film is 1.5nm.
Above-mentioned experimental result surface, the method using 3,4,9,10- tetracid dianhydride molecular film of single layer as seed layer,
It can be realized the sull that ultra-thin high quality is grown in two-dimensional material.
Its influence to the leakage current characteristic of FET device is verified below.
The hafnium oxide for growing 1.5nm, 4nm, 9nm and 15.6nm thickness on graphene respectively using the method for the present embodiment is thin
Then graphene double-gated devices are made in film, test the leakage data of the graphene double-gated devices of different hafnium oxide thickness, such as scheme
5a~5b.Wherein, Fig. 5 a is the breakdown indicatrix of the graphene double-gated devices of different hafnium oxide thickness；Fig. 5 b is statistics
The breakdown voltage and breakdown electric field of 30 graphene double-gated devices of different hafnium oxide thickness, it can be seen from the figure that breakdown potential
Pressure increases with equivalent oxide thickness, also linearly increasing, is carried by the highest to its linear fit, our available devices
Flowing sub- concentration is 6.5 × 1013cm-1；Breakdown electric field is quicklyd increase with the reduction of equivalent oxide thickness, highest breakdown electric field
It can achieve 15.5 megavolt per centimeters.Fig. 5 c is gate leak current face of 30 graphene double-gated devices when top-gated voltage is equal to 1 volt
Density, with the reduction of equivalent oxide thickness, gate leak current surface density is from 10-6Ampere/square centimeter is slowly increased；When equivalent
When oxidated layer thickness is 1 nanometer, gate leak current surface density is about 10-2Ampere/square centimeter still is able to meet low-power consumption
The requirement of electronic device.Illustrate that the sull of the method for the present invention preparation can still be kept excellent in the case where very thin
Different performance, the electronic device applications being applicable under diversified forms.
Embodiment 2
1) graphene two-dimensional layer material is prepared using mechanical stripping method, and graphene two-dimensional layer material is transferred to silicon
On piece；
2) 3,4,9,10- tetracid dianhydride powder are put into quartz boat, as growth source, and quartz boat are put into tubular type
Furnace center；Silicon wafer that transfer has graphene is placed on another quartz boat, and this quartz boat is put into quartz ampoule, and is held
The quartz boat of 3,4,9,10- tetracid dianhydride powder is at a distance of 2 centimetres；After placement, quartz ampoule is installed corresponding to tube furnace
Position, and vacuumize；
3) tube furnace is started, is warming up to 240 DEG C within furnace body temperature 10 minutes, then 260 DEG C is warming up within 5 minutes, at 260 DEG C
It maintains 0.8 hour, 3,4,9,10- tetracid dianhydride powder grow source evaporation, and deposit on graphene；It, will after heating
Tube furnace is naturally cooling to room temperature, terminates growth.
4) graphene of single layer 3,4,9,10- tetracid dianhydride molecular film moves to atomic layer from quartz ampoule growth
In deposition chamber, vacuum pumping is carried out to atomic layer deposition cavity, and cavity temperature is increased to 70 DEG C, wait 10min
Afterwards, then by cavity temperature 80 DEG C are increased to；
5) after cavity/cavity wall temperature reaches rated temperature, using four (dimethylamino) zirconiums as the metal of atomic layer deposition
Source, water set cycle-index as oxidation source, grow the zirconia film of 5nm thickness on the surface of graphene.
Fig. 6 is the atomic force microscope images for having grown the graphene of zirconium oxide, it is seen then that method of the invention can be realized
The zirconia film of ultra-thin high quality is grown in two-dimensional material.
Embodiment 3
1) graphene two-dimensional layer material is prepared using mechanical stripping method, and graphene two-dimensional layer material is transferred to silicon
On piece；
2) 3,4,9,10- tetracid dianhydride powder are put into quartz boat, as growth source, and quartz boat are put into tubular type
Furnace center；Silicon wafer that transfer has graphene is placed on another quartz boat, and this quartz boat is put into quartz ampoule, and is held
The quartz boat of 3,4,9,10- tetracid dianhydride powder is at a distance of 2 centimetres；After placement, quartz ampoule is installed corresponding to tube furnace
Position, and vacuumize；
3) tube furnace is started, is warming up to 240 DEG C within furnace body temperature 10 minutes, then 260 DEG C is warming up within 5 minutes, at 260 DEG C
It maintains 0.2 hour, 3,4,9,10- tetracid dianhydride powder grow source evaporation, and deposit on graphene；It, will after heating
Tube furnace is naturally cooling to room temperature, terminates growth.
4) graphene of single layer 3,4,9,10- tetracid dianhydride molecular film moves to atomic layer from quartz ampoule growth
In deposition chamber, vacuum pumping is carried out to atomic layer deposition cavity, and cavity temperature is increased to 80 DEG C, wait 10min
Afterwards, then by cavity temperature 90 DEG C are increased to；
5) after cavity/cavity wall temperature reaches rated temperature, using trimethyl aluminium as the source metal of atomic layer deposition, water is made
For oxidation source, cycle-index is set, grows the aluminum oxide film of 5nm thickness on the surface of graphene.
Fig. 7 is the atomic force microscope images for having grown the graphene of aluminium oxide, and illustrating can using method of the invention
Realize the aluminum oxide film that ultra-thin high quality is grown in two-dimensional material.
Embodiment 4
1) graphene two-dimensional layer material is prepared using mechanical stripping method, and graphene two-dimensional layer material is transferred to silicon
On piece；
2) 3,4,9,10- 4 formyl-2-imide powder are put into quartz boat, as growth source, and quartz boat are put into
Tube furnace center；The silicon wafer that transfer has graphene is placed on another quartz boat, and this quartz boat is put into quartz ampoule, with
The quartz boat of 3,4,9,10- 4 formyl-2-imide powder is held at a distance of 4 centimetres；After placement, quartz ampoule is installed to pipe
Formula furnace corresponding position, and vacuumize；
3) tube furnace is started, is warming up to 220 DEG C within furnace body temperature 10 minutes, then 240 DEG C is warming up within 5 minutes, at 240 DEG C
It maintains 0.8 hour, 3,4,9,10- 4 formyl-2-imide powder grow source evaporation, and deposit on graphene；Heating terminates
Afterwards, tube furnace is naturally cooling to room temperature, terminates growth.
4) graphene of single layer 3,4,9,10- 4 formyl-2-imide molecular film moves to original from quartz ampoule growth
In sublayer deposition chamber, vacuum pumping is carried out to atomic layer deposition cavity, and cavity temperature is increased to 70 DEG C, waited
After 5min, then cavity temperature is increased to 80 DEG C；
5) after cavity/cavity wall temperature reaches rated temperature, using trimethyl aluminium as the source metal of atomic layer deposition, water is made
For oxidation source, cycle-index is set, grows the aluminum oxide film of 3nm thickness on the surface of graphene.
Fig. 8 is the atomic force microscope images for having grown the graphene of aluminium oxide, it is seen then that with 3,4,9,10- tetra- formyls
Other organic dye molecule films such as diimine molecular film also can be realized as seed layer and grow excess of export in two-dimensional material
The sull of thin high quality.
Embodiment 5
1) molybdenum disulfide two-dimensional layer material is prepared using mechanical stripping method, and molybdenum disulfide two-dimensional layer material is shifted
Upper source-drain electrode is prepared onto silicon wafer, and in the two sides of molybdenum disulfide；Such as Fig. 9 (a), it is transferred to the thin layer on silicon wafer as substrate
Molybdenum disulfide with a thickness of 1.1nm.
2) 3,4,9,10- tetracid dianhydride powder are put into quartz boat, as growth source, and quartz boat are put into tubular type
Furnace center；The silicon wafer that transfer has molybdenum disulfide is placed on another quartz boat, and this quartz boat is put into quartz ampoule, with Sheng
The quartz boat of 3,4,9,10- tetracid dianhydride powder is put at a distance of 2cm；After placement, quartz ampoule is installed corresponding to tube furnace
Position, and vacuumize；
3) tube furnace is started, is warming up to 220 DEG C within furnace body temperature 10 minutes, then 240 DEG C is warming up within 5 minutes, at 240 DEG C
It maintains 0.8 hour, 3,4,9,10- tetracid dianhydride powder grow source evaporation, and deposit on molybdenum disulfide；After heating,
Tube furnace is naturally cooling to room temperature, terminates growth.
Fig. 9 (b) makes a living the atom of the thin layer molybdenum disulfide sample with single layer 3,4,9,10- tetracid dianhydride molecular film
Force microscope image, substrate surface molybdenum disulfide and monomolecular film with a thickness of 1.4nm, compared with Fig. 9 (a), Ke Yifa
Existing thickness increases 0.3nm, exactly single layer 3, the thickness of 4,9,10- tetracid dianhydride molecular films；It can from its surface topography
To find out, 3,4,9,10- tetracid dianhydride molecular film of single layer may be implemented uniformly to arrange on graphene.
4) molybdenum disulfide of single layer 3,4,9,10- tetracid dianhydride molecular film moves to atom from quartz ampoule growth
In layer deposition chamber, vacuum pumping is carried out to atomic layer deposition cavity, and cavity temperature is increased to 80 DEG C, wait 5min
Afterwards, then by cavity temperature 90 DEG C are increased to；
5) after cavity/cavity wall temperature reaches rated temperature, using four (dimethylamino) hafniums as the metal of atomic layer deposition
Source, water set cycle-index as oxidation source, in the hafnia film of molybdenum disulfide surface growth 1.5nm.
6) top-gated electrode is prepared on the molybdenum disulfide sample for grown hafnia film, and double grid survey is carried out to device
Examination.
Figure 10 is the atomic force microscope images for having grown the molybdenum disulfide of hafnium oxide.It can be seen that using of the invention
Method can prepare the hafnia film of uniform ground on molybdenum disulfide surface.
Figure 11 a is the transfer characteristic curve that the device molybdenum disulfide scans top-gated voltage under different back gate voltages.Figure 11 b
It is the transfer characteristic curve for further utilizing Figure 11 a, extracts the threshold value electricity under different back gate voltages in top-gated transfer characteristic curve
Pressure, draws out top-gated voltage-back gate voltage curve, therefrom ratio of the available top-gated capacitor to backgate capacitor, top-gated capacitor
Rate: backgate capacitivity is equal to 16.8, and since backgate is the aluminium oxide of 30nm, the dielectric constant of aluminium oxide is 7, then the hafnium oxide is thin
The equivalent oxide thickness of film is 1nm.The above results show to can be realized using method of the invention to be grown on molybdenum disulfide
The sull of ultra-thin high quality out.
Claims (10)
1. a kind of method for growing ultra-thin high quality oxide film on two-dimensional layer material, which is characterized in that including as follows
Step:
(1) single layer organic dye molecule film is grown on two-dimensional layer material using Van der Waals epitaxy growing technology；
(2) technique for atomic layer deposition is utilized, using the single layer organic dye molecule film as seed layer, in two-dimensional layer material
On grow the sull of ultra-thin homogeneous.
2. the method according to claim 1 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is that the two-dimensional layer material is graphene, black phosphorus, boron nitride or Transition-metal dichalcogenide.
3. the method according to claim 1 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is that the organic dye molecule film is 3,4,9,10- tetracid dianhydrides and its derivative, 3,4,9,10- tetra- formyls
Diimine and its derivative, rubrene and its derivative, N, any point in N- xylyl acid imide and its derivative
Sub- film.
4. the method according to claim 1 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is that the sull is that aluminum oxide film, hafnia film, zirconia film, thin film of titanium oxide or lanthana are thin
Film.
5. the method according to claim 1 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is, is growth source by substrate, organic dye molecule of two-dimensional layer material in step (1), spacing distance is placed in tube furnace
In, after tubular type stove evacuation, temperature is 240~260 DEG C, keeps the temperature 0.2~0.8h at heating furnace body to growth source position, makes to have
The evaporation of machine dye molecule, the organic dye molecule film to form single layer is deposited in two-dimensional layer material upper surface.
6. the method according to claim 5 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is, 2~4cm is spaced between the substrate and growth source and is placed.
7. the method according to claim 1 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is, in step (2), has the two-dimensional layer material of single layer organic dye molecule film to be transferred to atomic layer deposition chamber growth
It in body, vacuumizes, cavity temperature is increased to 80~90 DEG C, then passes to source metal and oxidation source, in two-dimensional layer material
Seed layer surface in situ deposits to obtain the sull of ultra-thin homogeneous.
8. the method according to claim 7 for growing ultra-thin high quality oxide film on two-dimensional layer material, special
Sign is, after vacuumizing, the temperature of the atomic layer deposition cavity is first increased to 70~80 DEG C, after waiting 5-10min, then will
Cavity temperature is increased to 80~90 DEG C.
9. the application that method described in claim 1 is used to prepare electronic device.
10. application according to claim 9, which is characterized in that the electronic device is field effect transistor, preparation side
Method includes the following steps:
(1) single layer organic dye molecule film is grown on two-dimensional layer material using Van der Waals epitaxy growing technology；
(2) technique for atomic layer deposition is utilized, using the single layer organic dye molecule film as seed layer, in two-dimensional layer material
On grow ultra-thin homogeneous sull, as dielectric layer；
(3) top-gated electrode is prepared on the two-dimensional layer material for grown ultrathin oxide film, obtains two-dimensional layer yard of material
Field effect transistor devices.
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