CN109402739A - A kind of two dimension bismuth oxygen selenium atom crystalline material, and its preparation method and application - Google Patents
A kind of two dimension bismuth oxygen selenium atom crystalline material, and its preparation method and application Download PDFInfo
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- CN109402739A CN109402739A CN201811566870.XA CN201811566870A CN109402739A CN 109402739 A CN109402739 A CN 109402739A CN 201811566870 A CN201811566870 A CN 201811566870A CN 109402739 A CN109402739 A CN 109402739A
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- crystalline material
- selenium atom
- bismuth oxygen
- bismuth
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- SYYDNLBOFQOSGT-UHFFFAOYSA-N [Bi]=O.[Se] Chemical group [Bi]=O.[Se] SYYDNLBOFQOSGT-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000002178 crystalline material Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000013078 crystal Substances 0.000 claims abstract description 59
- 239000011669 selenium Substances 0.000 claims abstract description 59
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 30
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 25
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 21
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 7
- 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 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000010445 mica Substances 0.000 claims description 12
- 229910052618 mica group Inorganic materials 0.000 claims description 12
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910052594 sapphire Inorganic materials 0.000 claims description 10
- 239000010980 sapphire Substances 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000011144 upstream manufacturing Methods 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 239000010410 layer Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 11
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010574 gas phase reaction Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 230000005669 field effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000005619 thermoelectricity Effects 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- YSCNMFDFYJUPEF-OWOJBTEDSA-N 4,4'-diisothiocyano-trans-stilbene-2,2'-disulfonic acid Chemical compound OS(=O)(=O)C1=CC(N=C=S)=CC=C1\C=C\C1=CC=C(N=C=S)C=C1S(O)(=O)=O YSCNMFDFYJUPEF-OWOJBTEDSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001803 electron scattering Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- 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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
-
- 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
-
- 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
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
Abstract
The present invention relates to a kind of preparation methods of two-dimentional bismuth oxygen selenium atom crystal, it the described method comprises the following steps: physical vapour deposition (PVD) will be carried out containing the presoma of bismuth element and selenium element, two-dimentional bismuth oxygen selenium atom crystalline material is obtained, the two dimension bismuth oxygen selenium atom crystalline material is tetragonal crystal system.The present invention uses physical vapour deposition (PVD), solve the problems, such as that the proportion of bismuth source and selenium source is not easy to control in chemical gas phase reaction process, obtained two-dimentional bismuth oxygen selenium atom crystalline material purity is higher, and vacancy defect is less, and then electron mobility is higher, electron mobility >=135cm2/ (Vs), while relative to chemical vapor deposition, physical vapour deposition (PVD) may make two-dimentional bismuth oxygen selenium atom crystalline material crystal form integrality higher, crystalline size is bigger, single crystal domains side length can reach a millimeter rank, maximum single crystal domains side length >=1.7mm, minimum single crystal domains side length >=200 μm.
Description
Technical field
The invention belongs to two-dimensional material fields, and in particular to a kind of two dimension bismuth oxygen selenium atom crystalline material and its preparation side
Method and purposes.
Background technique
The progress of modern information technologies is largely dependent upon with integrated circuit that semiconductor silicon is basic material
Development.Currently, due to being limited by from the physics laws such as short-channel effect and manufacturing cost, main stream of CMOS (complementary metal
Oxide semiconductor) technology is to be up to the technology node of 10nm, it is difficult to continue to lift up, this also implies that " Moore's Law " may
Face termination.Therefore, the transistor technology of novel channel material and new principle is explored, to substitute silicon substrate CMOS technology, always
Since be scientific circles and industrial circle one of mainstream research direction.
Simultaneously, it is contemplated that semiconductor material is in practical extensive and high degree of enrichment application demand, the growth of large area material
It prepares particularly important；Since crystal boundary existing between domain will cause a large amount of electron scatterings, just necessarily require to obtain large scale list
Brilliant growth is prepared number of grain boundaries is effectively reduced.Compared to the TMDCs (transition metal of the lower electron mobility of Centimeter Level monocrystalline
Sulfide) material, Bi2O2This kind of semiconductor material of the Se band gap and high stability big due to the electron mobility of its superelevation, low
Excellent properties are shown in terms of warm Quantum Transport device and field effect transistor.The material is expected to after graphene, molybdenum disulfide, black
After stars' two-dimensional material such as phosphorus, become the completely new channel material for being rich in competitiveness, however there is presently no effective preparation is high
Quality Bi2O2The method of Se monocrystalline.
CN108039403A discloses a kind of mass preparation of high quality wafer scale selenium bismuth oxide semiconductor single crystal thin film
Method, described method includes following steps: being growth with single crystal wafers using the compound containing Bi element and Se element as raw material
Substrate carries out chemical vapor deposition, obtains the Bi2O2Se film.The method process flow is simple, but anti-in chemical gaseous phase
The proportion of bismuth source and selenium source is not easy to control during answering, and the crystal percentage being prepared is not fixed, while easily being produced in plane of crystal
Raw a large amount of selenium vacancy, is not able to satisfy the demand of high-quality semiconductor material, at the same chemical vapor deposition be made crystalline size compared with
Small is 100 μm.
CN106011783B discloses a kind of high mobility stratiform Bi2O2Se semiconductive thin film and preparation method thereof, the side
Method includes the following steps: with Bi2O3Powder and Bi2Se3Block is raw material, and chemical vapor deposition is carried out in mica substrate, deposition
After obtain layered Bi2O2Se semiconductive thin film.The method is simple and easy, but the crystal percentage being prepared is not
It is fixed, while it being also easy to produce a large amount of selenium vacancy in plane of crystal, it is not able to satisfy the demand of high-quality semiconductor material, while chemistry
Being vapor-deposited and smaller crystalline size is made is 100 μm.
CN104261357B discloses a kind of Bi2O2Se base thermoelectricity material and preparation method thereof, the method includes walking as follows
It is rapid: to press Bi2-xSnxO2The stoichiometric ratio of Se (0≤x≤0.10) weighs Bi2O3, Bi, Se and SnO2Powder, carried out after mixing
Vacuum sealing tube, calcining, complete object phase at the phase stage；Calcined powder is compacted, is sintered using SPS discharge plasma,
Obtain the Bi of pure phase and Sn doping2O2Se base thermoelectricity material.The method is simple and easy, but the plane of crystal being prepared is easy
A large amount of selenium vacancy is generated, is not able to satisfy the demand of high-quality semiconductor material.
Therefore, this field needs to develop a kind of preparation method of high-quality bismuth oxygen selenium monocrystalline two-dimensional material, and preparation process
Simply, can industrialized production, the bismuth oxygen selenium monocrystalline two-dimensional material macro-size being prepared is larger, for playing it in high-performance
Field of electronic devices has important meaning.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of two-dimentional bismuth oxygen selenium atom crystalline materials
Preparation method, the described method comprises the following steps:
Physical vapour deposition (PVD) will be carried out containing the presoma of bismuth element and selenium element, obtains two-dimentional bismuth oxygen selenium atom crystal material
Material.
The present invention uses physical vapour deposition (PVD), and it is not easily-controllable to solve the proportion of bismuth source and selenium source in chemical gas phase reaction process
The problem of processed, obtained two-dimentional bismuth oxygen selenium atom crystalline material purity is higher, and vacancy defect is less, and then electron mobility is more
Height, electron mobility >=135cm2/ (Vs), while relative to chemical vapor deposition, physical vapour deposition (PVD) may make two dimension
Bismuth oxygen selenium atom crystalline material crystal form integrality is higher, and crystalline size is bigger, and single crystal domains side length can reach a millimeter rank, maximum single
Domain side length >=1.7mm, minimum single crystal domains side length >=200 μm.
Preparation method of the invention can realize the size controllable preparation of two-dimentional bismuth oxygen selenium atom crystalline material, and preparation process
Simply, operation is easy, and preparation cost is low, is suitable for industrialized production.
Preferably, the presoma containing bismuth element and selenium element is Bi2O2Se powder.
Preferably, the physical vapour deposition (PVD) carries out in growth substrates.
Preferably, the growth substrates include at least one substrate.
Preferably, the substrate is single crystal substrates, preferably any in mica substrate, sapphire substrates and strontium titanate base bottom
It is a kind of or at least two combination.
Mica substrate of the present invention is the fresh mica substrate after removing, substrate of the present invention and Bi2O2The lattice of Se
Matching is good, carries out physical vapour deposition (PVD) on the substrate, has the crystal that can obtain high quality and can realize large area
The advantages that growth.
Preferably, the sapphire substrates are A surface sapphire substrate and/or R surface sapphire substrate.
Preferably, the strontium titanate base bottom is strontium titanate base bottom (100) face, strontium titanate base bottom (110) face and strontium titanate base
In bottom (111) face any one or at least two combination.
Preferably, physical vapour deposition (PVD) of the present invention the following steps are included:
Presoma containing bismuth element and selenium element is placed in the airflow direction upstream end region of reacting furnace, growth substrates are placed in
The airflow direction downstream end regions of reacting furnace, under protective gas environment to the presoma containing bismuth element and selenium element into
Reaction system natural cooling it is former to be obtained two-dimentional bismuth oxygen selenium under conditions of being passed through protective gas after heat treatment by row heat treatment
Sub- crystalline material.
Preferably, protective gas of the present invention include in nitrogen, argon gas, helium and neon any one or at least
Two kinds of combination, preferably nitrogen.
Preferably, the reacting furnace includes horizontal pipe furnace.
Preferably, the presoma containing bismuth element and selenium element is 5cm~10cm at a distance from growth substrates, preferably
6cm, such as 6cm, 7cm, 8cm, 9cm etc..
Preferably, the heating rate of the heat treatment is 20 DEG C/min~40 DEG C/min, preferably 30 DEG C/min, such as 25
DEG C/min, 30 DEG C/min, 35 DEG C/min etc..
Preferably, the temperature of the heat treatment is 580 DEG C~800 DEG C, such as 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C, 780
DEG C etc..
Preferably, the time of the heat treatment be 5min~30min, such as 8min, 10min, 15min, 20min,
25min, 28min etc..
Preferably, the protective gas be passed through rate be 50sccm~300sccm, preferably 200sccm, such as
80sccm, 100sccm, 150sccm, 180sccm, 200sccm, 250sccm etc..
Preferably, the temperature of the natural cooling is 20 DEG C~30 DEG C, preferably 25 DEG C, such as 21 DEG C, 22 DEG C, 23 DEG C, 24
DEG C, 25 DEG C, 26 DEG C, 27 DEG C, 28 DEG C, 29 DEG C etc..
As optimal technical scheme, a kind of preparation method of two-dimentional bismuth oxygen selenium atom crystalline material of the present invention is described
Preparation method includes the following steps:
By Bi2O2Se powder is placed in the airflow direction upstream end region of horizontal pipe furnace, and mica substrate is placed in the gas of reacting furnace
Flow direction downstream end regions, Bi2O2Se powder is 6cm at a distance from mica substrate, under nitrogen gas environment, with 30 DEG C/min
Heating rate rises to 580 DEG C~800 DEG C, to Bi2O2Se powder is heat-treated 5min~30min, is passed through after heat treatment in nitrogen gas
Under conditions of rate is 200sccm, reaction system is naturally cooled to 25 DEG C, obtains two-dimentional bismuth oxygen selenium atom crystalline material.
The second object of the present invention is to provide a kind of two-dimentional bismuth oxygen selenium atom crystalline material, the two dimension bismuth oxygen selenium atom is brilliant
Body material is obtained by a kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material described in the first purpose.
The two-dimentional bismuth oxygen selenium atom crystalline material size that the present invention is prepared is larger, bismuth element in crystal, oxygen element and
Selenium element distributing homogeneity is preferable, and being constructed photodetector has many advantages, such as to respond fast, high sensitivity.
Preferably, the pattern of the two-dimentional bismuth oxygen selenium atom crystalline material is quadrangle sheet.
Preferably, the crystallographic system of the two-dimentional bismuth oxygen selenium atom crystalline material is tetragonal crystal system.
Preferably, the molecular formula of the two-dimentional bismuth oxygen selenium atom crystalline material is Bi2O2Se。
Preferably, 200 μm of side length > of the two-dimentional bismuth oxygen selenium atom crystal single crystal domains, for example, 500 μm, 800 μm, 1mm,
2mm etc..
The side length for the two-dimentional bismuth oxygen selenium atom crystalline material single crystal domains that the present invention is prepared is larger, in the prior art
Micron level, the side length of present invention two dimension bismuth oxygen selenium atom crystalline material can reach a millimeter rank.
Preferably, the two-dimentional bismuth oxygen selenium atom crystalline material with a thickness of 0.62nm~10nm, such as 0.7nm,
1.2nm, 3.6nm, 4.8nm, 5.2nm, 6.6nm, 7.8nm, 8.3nm, 9.6nm etc..
Preferably, the number of plies of the two-dimentional bismuth oxygen selenium atom crystalline material is single layer, bilayer or few layer.
The third object of the present invention is to provide a kind of purposes of bismuth oxygen selenium atom crystalline material two-dimentional as described in the second purpose,
The two dimension bismuth oxygen selenium atom crystalline material is for any one in micro-nano electronic device, optical device and chemical biosensor
Kind or at least two combination.
Compared with prior art, the invention has the following beneficial effects:
(1) present invention uses physical vapour deposition (PVD), solves in chemical gas phase reaction process the proportion of bismuth source and selenium source not
Manageable problem, obtained two-dimentional bismuth oxygen selenium atom crystalline material purity is higher, and vacancy defect is less, and then electron mobility
It is higher, electron mobility >=135m2/ (Vs), while relative to chemical vapor deposition, physical vapour deposition (PVD) may make two dimension
Bismuth oxygen selenium atom crystalline material crystal form integrality is higher, and the size that crystal is made is bigger, and single crystal domains side length can reach a millimeter rank,
Maximum single crystal domains side length >=1.7mm, minimum single crystal domains side length >=200 μm.
(2) preparation method of the invention can realize the size controllable preparation of two-dimentional bismuth oxygen selenium atom crystalline material, and prepare
Simple process, operation are easy, and preparation cost is low, are suitable for industrialization production.
(3) bismuth element, oxygen element and selenium element distribution in the two-dimentional bismuth oxygen selenium atom crystalline material that the present invention is prepared
Uniformity is preferable, and being constructed photodetector has many advantages, such as to respond fast, high sensitivity.
Detailed description of the invention
Fig. 1 (a-b) is the optical microscope picture for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 2 is the atomic force microscope images for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 3 is Raman spectrum of the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared of embodiment 1 under 532nm laser
Figure；
Fig. 4 (a-c) is the photoelectron spectroscopy test chart for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 5 a is the low power transmission electron microscope figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 5 b is the high power transmission electron microscope figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 5 c is the selective electron diffraction figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 6 a is the transmission electron microscope angle of elevation annular for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared
Dark field image；
Fig. 6 b is the bismuth element Surface scan figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 6 c is the oxygen element Surface scan figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Fig. 6 d is the selenium element Surface scan figure for the two-dimentional bismuth oxygen selenium atom crystalline material that embodiment 1 is prepared；
Difference constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that Fig. 7 is prepared for embodiment 1 links up the field effect of width
Answer the drain current versus drain voltage curve of transistor；
Fig. 8 be embodiment 1 prepare two-dimentional bismuth oxygen selenium atom crystalline material constructed by photodetector 660nm laser not
With the photoelectric respone figure under power；
Fig. 9 is photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material of the preparation of embodiment 1 under 660nm laser
Electric current and time plot；
Figure 10 is photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material of the preparation of embodiment 1 in 660nm laser
Under opening time and shut-in time；
Figure 11 is photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material of the preparation of embodiment 1 in 660nm laser
The responsiveness and detectivity correlated performance of lower calculating；
Figure 12 is the device figure that embodiment 1 prepares two-dimentional bismuth oxygen selenium atom crystalline material.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
A kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material includes the following steps:
By Bi2O2Se powder is placed in the airflow direction upstream end region of horizontal pipe furnace, and mica substrate is placed in the gas of reacting furnace
Flow direction downstream end regions, Bi2O2Se powder is 6cm at a distance from mica substrate, under nitrogen gas environment, with 30 DEG C/min
Heating rate rises to 620 DEG C, to Bi2O2Se powder is heat-treated 25min, and being passed through rate in nitrogen gas after heat treatment is 200sccm
Under conditions of, reaction system is naturally cooled to 25 DEG C, obtains two-dimentional bismuth oxygen selenium atom crystalline material test result such as Fig. 1~12
It is shown.
Fig. 1 a, 1b are the optical microscope picture for the two-dimentional bismuth oxygen selenium atom crystalline material being prepared, can be with by Fig. 1 a
Find out that crystal is quadrangle sheet, crystal single crystal domains side length is enriched in 300 μm, and Fig. 1 b is crystalline material maximum single crystal domains side length
2mm；
Fig. 2 is the atomic force microscope images for the two-dimentional bismuth oxygen selenium atom crystalline material being prepared, as seen from the figure
The material of crystal with a thickness of 0.62nm and 1.2nm, obtain different layers of two-dimentional bismuth oxygen selenium atom crystalline materials；
Fig. 3 is the Raman spectrogram of the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared under 532nm laser, You Tuke
Meet bismuth oxygen selenium vibration absorption peak to find out；
Fig. 4 (a-c) is the test result figure of the photoelectron spectroscopy for the two-dimentional bismuth oxygen selenium atom crystalline material being prepared, by
Figure is it can be seen that Bi element, Se element and O element all meet the energy band in bismuth oxygen selenium crystal structure；
Fig. 5 a is the low power transmission electron microscope picture for the two-dimentional bismuth oxygen selenium atom crystalline material being prepared, and Fig. 5 b is
High power transmission electron microscope picture can be seen that have obtained the sample of high quality by this two width figure, and Fig. 5 c is two-dimentional bismuth oxygen selenium
The selective electron diffraction figure of atomic crystal material, tetragonal crystal system is presented in sample as seen from the figure；
Fig. 6 a is the transmission electron microscope angle of elevation annular dark for the two-dimentional bismuth oxygen selenium atom crystalline material being prepared,
Fig. 6 b is the bismuth element Surface scan picture of two-dimentional bismuth oxygen selenium atom crystalline material, and bismuth element is evenly distributed as seen from the figure, figure
6c is the oxygen element Surface scan picture of two-dimentional bismuth oxygen selenium atom crystalline material, and oxygen element is evenly distributed as seen from the figure, Fig. 6 d
For the selenium element Surface scan picture of two-dimentional bismuth oxygen selenium atom crystalline material, selenium element is evenly distributed as seen from the figure；
Fig. 7 is field effect transistor constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared in different communication width
Under drain current versus drain voltage curve, by the figure can be seen that device present Ohmic contact；
Fig. 8 is that photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared is different in 660nm laser
Photoelectric respone figure under power can be seen that Ohmic contact, and photoelectric current constantly mentioning with power is presented in device by the figure
It is high and increase；
Fig. 9 is photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared under 660nm laser
Electric current and time plot can be seen that preferable stability is presented in device by the figure；
Figure 10 is photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared under 660nm laser
Opening time and shut-in time can be seen that the response time is short by the figure, open 6ms and close 20ms；
Figure 11 is that photodetector constructed by the two-dimentional bismuth oxygen selenium atom crystalline material that is prepared is counted under 660nm laser
The responsiveness and detectivity correlated performance of calculation, response is fast, high sensitivity；
Figure 12 is the reaction unit figure that embodiment 1 prepares two-dimentional bismuth oxygen selenium atom crystalline material.
Embodiment 2
The difference from embodiment 1 is that the temperature of heat treatment is 580 DEG C.
Embodiment 3
The difference from embodiment 1 is that the temperature of heat treatment is 800 DEG C.
Embodiment 4
The difference from embodiment 1 is that the time of heat treatment is 5min.
Embodiment 5
The difference from embodiment 1 is that the time of heat treatment is 30min.
Embodiment 6
A kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material includes the following steps:
By Bi2O2Se powder is placed in the airflow direction upstream end region of horizontal pipe furnace, and A surface sapphire substrate is placed in reaction
The airflow direction downstream end regions of furnace, Bi2O2Se powder is 5cm at a distance from A surface sapphire substrate, under argon gas environment,
620 DEG C are risen to 20 DEG C/min heating rate, to Bi2O2Se powder is heat-treated 25min, is passed through speed in argon gas after heat treatment
Under conditions of rate is 50sccm, reaction system is naturally cooled to 20 DEG C, obtains two-dimentional bismuth oxygen selenium atom crystalline material.
Embodiment 7
A kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material includes the following steps:
By Bi2O2Se powder is placed in the airflow direction upstream end region of horizontal pipe furnace, and strontium titanate base bottom (100) face is placed in
The airflow direction downstream end regions of reacting furnace, Bi2O2Se powder is 10cm at a distance from strontium titanate base bottom (100) face, in argon gas gas
Under body environment, 620 DEG C are risen to 40 DEG C/min heating rate, to Bi2O2Se powder is heat-treated 25min, in argon gas gas after heat treatment
Body is passed through rate reaction system to be naturally cooled to 30 DEG C, obtains two-dimentional bismuth oxygen selenium atom crystal material under conditions of 300sccm
Material.
Comparative example 1
It is comparative example with embodiment 1 in CN106011783B, preparation method includes the following steps:
Weigh 0.71 gram of Bi2O3Powder and 1.00 grams of Bi2Se3Block (molar ratio 1:1) places it in tube furnace quartz ampoule
Center, fluorophologopite substrate is placed at the downstream at 10~14 centimetres of tube furnace center.It is passed through carrier gas argon gas, maintains body
Be pressure be 200 supports.Temperature is risen to 630 degrees Celsius, is maintained 5 minutes, chemical vapor deposition is carried out.Stop carrying after deposition
Being passed through for gas, is naturally cooling to room temperature, will be deposited with Bi2O2The mica substrate of Se film is taken out, and stratiform Bi is obtained2O2Se is partly led
Body thin film.
Performance test:
The two-dimentional bismuth oxygen selenium atom crystalline material being prepared is performed the following performance tests:
(1) single crystal domains side length is tested: being tested using optical microscopy, the two dimension being prepared in each example
In bismuth oxygen selenium atom crystalline material, the maximum bismuth oxygen selenium atom crystal of single crystal domains side length and the smallest bismuth oxygen selenium of single crystal domains side length are taken
Atomic crystal is tested.
(2) electron mobility is tested: first by two-dimentional bismuth oxygen selenium atom crystalline material obtained in semiconductor probe platform instrument
Device, atmosphere and carries out device detection at room temperature, obtains i-v curve, finally according to electron mobility formula μ=L/ (W ×
(ε0εr/d)×Vds)×dIds/dVgsThe electron mobility of material is calculated.
Table 1
| Maximum single crystal domains side length | Minimum single crystal domains side length | Electron mobility cm2/(V·s) | |
| Embodiment 1 | 2mm | 210μm | 150 |
| Embodiment 2 | 1.9mm | 201μm | 148 |
| Embodiment 3 | 1.8mm | 203μm | 145 |
| Embodiment 4 | 1.9mm | 205μm | 140 |
| Embodiment 5 | 1.7mm | 200μm | 135 |
| Embodiment 6 | 1.8mm | 200μm | 138 |
| Embodiment 7 | 1.9mm | 203μm | 142 |
| Comparative example 1 | 100μm | 20μm | 100 |
It can be seen from Table 1 that 1-7 of the embodiment of the present invention, the single crystal domains side length of material is made using physical vapour deposition (PVD)
It is larger, maximum single crystal domains side length >=1.7mm, minimum single crystal domains side length >=200 μm, electron mobility >=135cm2/(V·s)。
It can be seen from Table 1 that comparative example 1 is relative to the maximum single crystal domains side length of embodiment 1, minimum single crystal domains side length and electricity
Transport factor is smaller, it may be possible to since comparative example 1 prepares bismuth oxygen selenium atom crystalline material, chemical gas using chemical vapour deposition technique
In phase sedimentation preparation process, the proportion of bismuth source and selenium source is not easy to control, the two dimension bismuth oxygen selenium atom crystalline material obtained from
Surface is easy to produce a large amount of selenium vacancy, and electron mobility is lower, while the crystal form integrality of crystal is made in chemical vapor deposition
Lower, size is smaller, so comparative example 1 is relative to the maximum single crystal domains side length of embodiment 1, minimum single crystal domains side length and electron transfer
Rate is smaller.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material, which is characterized in that the described method comprises the following steps:
Physical vapour deposition (PVD) will be carried out containing the presoma of bismuth element and selenium element, obtains two-dimentional bismuth oxygen selenium atom crystalline material.
2. preparation method as described in claim 1, which is characterized in that the presoma containing bismuth element and selenium element is
Bi2O2Se powder.
3. preparation method as claimed in claim 1 or 2, which is characterized in that the physical vapour deposition (PVD) is enterprising in growth substrates
Row；
Preferably, the growth substrates include at least one substrate；
Preferably, the substrate is single crystal substrates, preferably any one in mica substrate, sapphire substrates and strontium titanate base bottom
Or at least two combination；
Preferably, the sapphire substrates are A surface sapphire substrate and/or R surface sapphire substrate；
Preferably, the strontium titanate base bottom is strontium titanate base bottom (100) face, strontium titanate base bottom (110) face and strontium titanate base bottom
(111) any one in face or at least two combination.
4. the preparation method as described in one of claim 1-3, which is characterized in that the physical vapour deposition (PVD) includes following step
It is rapid:
Presoma containing bismuth element and selenium element is placed in the airflow direction upstream end region of reacting furnace, growth substrates are placed in reaction
The airflow direction downstream end regions of furnace carry out heat containing bismuth element and the presoma of selenium element to described under protective gas environment
Reaction system natural cooling it is brilliant to be obtained two-dimentional bismuth oxygen selenium atom under conditions of being passed through protective gas after heat treatment by processing
Body material.
5. the preparation method as described in one of claim 1-4, which is characterized in that the protective gas include nitrogen, argon gas,
In helium and neon any one or at least two combination, preferred nitrogen；
Preferably, the reacting furnace includes horizontal pipe furnace；
Preferably, the presoma containing bismuth element and selenium element is 5cm~10cm, preferably 6cm at a distance from growth substrates；
Preferably, the heating rate of the heat treatment is 20 DEG C/min~40 DEG C/min, preferably 30 DEG C/min；
Preferably, the temperature of the heat treatment is 580 DEG C~800 DEG C；
Preferably, the time of the heat treatment is 5min~30min；
Preferably, the rate that is passed through of the protective gas is 50sccm~300sccm, preferably 200sccm；
Preferably, the temperature of the natural cooling is 20 DEG C~30 DEG C, preferably 25 DEG C.
6. the preparation method of the two-dimentional bismuth oxygen selenium atom crystalline material as described in one of claim 1-5, which is characterized in that described
Preparation method includes the following steps:
By Bi2O2Se powder is placed in the airflow direction upstream end region of horizontal pipe furnace, and mica substrate is placed in the air-flow side of reacting furnace
Downstream end region, Bi2O2Se powder is 6cm at a distance from mica substrate, under nitrogen gas environment, with 30 DEG C/min heating
Rate rises to 580 DEG C~800 DEG C, to Bi2O2Se powder is heat-treated 5min~30min, is passed through rate in nitrogen gas after heat treatment
Under conditions of 200sccm, reaction system is naturally cooled to 25 DEG C, obtains two-dimentional bismuth oxygen selenium atom crystalline material.
7. a kind of two dimension bismuth oxygen selenium atom crystalline material, which is characterized in that the two dimension bismuth oxygen selenium atom crystalline material passes through power
Benefit requires a kind of preparation method of two dimension bismuth oxygen selenium atom crystalline material described in one of 1-6 to obtain.
8. two dimension bismuth oxygen selenium atom crystalline material as claimed in claim 7, which is characterized in that the two dimension bismuth oxygen selenium atom is brilliant
The pattern of body material is quadrangle sheet；
Preferably, the crystallographic system of the two-dimentional bismuth oxygen selenium atom crystalline material is tetragonal crystal system；
Preferably, the molecular formula of the two-dimentional bismuth oxygen selenium atom crystalline material is Bi2O2Se。
9. two dimension bismuth oxygen selenium atom crystalline material as claimed in claim 7 or 8, which is characterized in that the two dimension bismuth oxygen selenium is former
200 μm of the side length > of sub- crystal single crystal domains；
Preferably, the two-dimentional bismuth oxygen selenium atom crystalline material with a thickness of 0.62nm~10nm；
Preferably, the number of plies of the two-dimentional bismuth oxygen selenium atom crystalline material is single layer, bilayer or few layer.
10. a kind of purposes of bismuth oxygen selenium atom crystalline material two-dimentional as described in one of claim 7-9, which is characterized in that described
Two-dimentional bismuth oxygen selenium atom crystalline material in micro-nano electronic device, optical device and chemical biosensor any one or
At least two combination.
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