CN105463580B - Preparation method of cadmium selenide or cadmium sulfide two-dimensional single crystal nanosheet - Google Patents
Preparation method of cadmium selenide or cadmium sulfide two-dimensional single crystal nanosheet Download PDFInfo
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000013078 crystal Substances 0.000 title claims abstract description 33
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000002135 nanosheet Substances 0.000 title abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 61
- 239000010445 mica Substances 0.000 claims abstract description 44
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 44
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 19
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 27
- 239000002055 nanoplate Substances 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910021389 graphene Inorganic materials 0.000 claims description 13
- 238000011144 upstream manufacturing Methods 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 8
- 238000010494 dissociation reaction Methods 0.000 claims description 4
- 230000005593 dissociations Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 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
- 239000010453 quartz Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- RBORURQQJIQWBS-QVRNUERCSA-N (4ar,6r,7r,7as)-6-(6-amino-8-bromopurin-9-yl)-2-hydroxy-2-sulfanylidene-4a,6,7,7a-tetrahydro-4h-furo[3,2-d][1,3,2]dioxaphosphinin-7-ol Chemical compound C([C@H]1O2)OP(O)(=S)O[C@H]1[C@@H](O)[C@@H]2N1C(N=CN=C2N)=C2N=C1Br RBORURQQJIQWBS-QVRNUERCSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 239000012159 carrier gas Substances 0.000 abstract description 11
- 238000011160 research Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 230000005669 field effect Effects 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 229910052711 selenium Inorganic materials 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 11
- 239000002086 nanomaterial Substances 0.000 description 11
- 238000000407 epitaxy Methods 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 5
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 239000011669 selenium Substances 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 238000003776 cleavage reaction Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 230000007017 scission Effects 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- -1 Cadmium Chalcogenide Chemical class 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 description 1
- 229910000238 buergerite Inorganic materials 0.000 description 1
- AQCDIIAORKRFCD-UHFFFAOYSA-N cadmium selenide Chemical compound [Cd]=[Se] AQCDIIAORKRFCD-UHFFFAOYSA-N 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- QYFRTHZXAGSYGT-UHFFFAOYSA-L hexaaluminum dipotassium dioxosilane oxygen(2-) difluoride hydrate Chemical compound O.[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O QYFRTHZXAGSYGT-UHFFFAOYSA-L 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 238000012795 verification Methods 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
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
-
- 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
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
- C30B29/50—Cadmium sulfide
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Photovoltaic Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of cadmium selenide or cadmium sulfide two-dimensional single crystal nanosheets. The method adopts Van der Waals epitaxial growth technology to prepare CdSe or CdS two-dimensional single crystal nano-sheets, and is characterized in that mica sheets with smooth surfaces and no chemical dangling bonds are adoptedAs a substrate, CdCl2CdCl under high-temp condition with powder, Se powder or S powder as source and argon as carrier gas2The vapor reacts with Se or S vapor to form CdSe or CdS vapor, and then the CdSe or CdS vapor is deposited on a mica sheet to form nuclei and epitaxially grows into a CdSe or CdS two-dimensional single crystal nanosheet. The method is simple to operate, low in cost and strong in controllability, and the obtained CdSe or CdS has the advantages of good size uniformity, high crystallinity and the like, and has important research value and wide application prospect in the fields of solar cells, field effect transistors, photoelectric detectors, photocatalysis and the like.
Description
Technical field
The present invention relates to nanometer semiconductor technology field.More particularly, to a kind of large area cadmium selenide (CdSe) and sulphur
The preparation method of cadmium (CdS) two dimension single crystal nanoplate.
Background technology
In recent years, two-dimension nano materials cause the research in global range with its unique structure and physicochemical characteristics
Upsurge, huge application potential has been shown in basic research and field of industrial production.The widest two-dimentional material of research at present
Stratified material of the material mainly based on graphene and Transition-metal dichalcogenide.Graphene has that intensity is big, carrier moves
The advantages that shifting rate is high, but intrinsic graphene band gap is zero, result in based on its field-effect transistor current switch it is less efficient.
The Transition-metal dichalcogenide of stratiform is similar to graphene-structured, since the weaker model ylid bloom action power of interlayer is conducive to it
Peel off as ultra-thin two-dimensional nanostructure.The property that Transition-metal dichalcogenide two-dimension nano materials are shown is certain
It compensate for the deficiency of graphene in degree, there is the regulatable band gap of 1-2eV.Such as molybdenum disulfide, tungsten disulfide etc., when its by
When bulk is changed into single layer configuration, its band gap can be direct band gap from indirect band gap transitions, this causes it in electronics and photoelectron
Have in field sizable application prospect (Q.H.Wang, Kourosh Kalantar-Zadeh, Andras Kis,
Jonathan N.Coleman and Michael S.Strano.Electronics and optoelectronics of
two-dimensional transition metal dichalcogenides.Nature Nanotechnology,2012,
7,699-712)。
However, much the non-laminar materials with excellent specific property due to the limitation of its crystal structure, lack two dimension respectively to
The driving force of anisotropic growth, so the two-dimensional nanostructure for preparing non-laminar material has very big challenge.Recent study
Show, the two-dimensional structure of non-laminar material has prepared very big progress.Scientists are using Van der Waals epitaxy technology priority
Prepared the materials such as tellurium, GaAs, perovskite two-dimensional nano sheet structure (Q.S.Wang, M.Safdar, K.Xu,
M.Mirza,Z.X.Wang,and J.He.Van der Waals Epitaxy and Photoresponse of
Hexagonal Tellurium Nanoplates on Flexible Mica Sheets.ACS Nano,2014,8,7497-
7505；Y.Alaskar,S.Arafin,D.Wickramaratne,M.A.Zurbuchen,L.He,J.McKay,Q.Lin,
M.S.Goorsky,R.K.Lake,K.L.Wang.Towards van der Waals Epitaxial Growth of GaAs
on Si using a Graphene Buffer Layer.Adv.Funct.Mater.2014,24,6629-6638；
Y.P.Wang,Y.F.Shi,G.Q.Xin,J.Lian,and J.Shi,Two-Dimensional van der Waals
Epitaxy Kinetics in a Three-Dimensional Perovskite Halide.Cryst.Growth
Des.2015,15,4741-4749.).The successful preparation of these non-laminar material two-dimensional nanostructures enriches two-dimensional material
Database, also provides possibility for its application in the fields such as solar cell, transistor, photodetector.
At present, preparing the method for two-dimensional nanostructure mainly has top-down stripping method and vapour deposition from bottom to top
Method.Van der Waals epitaxy technology is a kind of unique CVD method, and prepares non-laminar material two-dimensional nanostructure now
One of most common method.Van der Waals epitaxy technology generally use surface is smooth and material without chemical dangling bond is as substrate, profit
The two-dimensional material of high quality is prepared with the Van der Waals force between epitaxial layer and substrate or electrostatic weak interaction.This technology without
Need epitaxial layer and substrate bonding, the strain energy of epitaxial layer quickly and efficiently relaxation, so as to effectively reduce epitaxial layer and substrate is brilliant
The influence of lattice mismatch, is particularly suitable for growth (the Muhammad Iqbal Bakti of the material big with substrate lattice mismatch
Utama, Q.Zhang, J.Zhang, Y.W.Yuan, Francisco J.Belarre, Jordi Arbiolbc and
Q.H.Xiong.Recent Developments and Future Directions in the Growth of
Nanostructures by van der Waals Epitaxy.Nanoscale 2013,5,3570–3588.).At present, model
Moral China epitaxy technology reaches its maturity, and be widely used in stratified material two-dimensional structure growth (S.Najmaei, Z.Liu,
W.Zhou,X.L.Zou,G.Shi,S.D.Lei,B.I.Yakobson,J.C.Idrobo,P.M.Ajayan and
J.Lou.Vapour phase growth and grain boundary structure of molybdenum
Disulphide atomic layers.Nat.Mater.2013,12,754-759.), the preparation of two-dimensional hetero-junction
(X.W.Zhang,F.Meng,Jeffrey R.Christianson,Christian Arroyo-Torres,Mark
A.Lukowski,D.Liang,J.R.Schmidt,and S.Jin.Vertical Heterostructures of Layered
Metal Chalcogenides by van der Waals Epitaxy.Nano Lett.2014,14,3047-3054), with
And non-laminar material it is one-dimensional (M.I.B.Utama, Z.P.Peng, R.Chen, B.Peng, X.L.Xu, Y.J.Dong,
L.M.Wong,S.J.Wang,H.D.Sun and Q.H.Xiong.Vertically Aligned Cadmium
Chalcogenide Nanowire Arrays on Muscovite Mica:A Demonstration of Epitaxial
Growth Strategy.Nano Lett.2011,11,3051-3057.) and two-dimensional structure growth (Q.S.Wang, K.Xu,
Z.X.Wang,F.Wang,Y.Huang,M.Safdar,X.Y.Zhan,F.M.Wang,Z.Z.Cheng,J.He,van der
Waals Epitaxial Ultrathin Two-Dimensional Nonlayered Semiconductor for Highly
Efficient Flexible Optoelectronic Devices.Nano Lett.2015,15,1183-1189.).However,
Up to the present other non-laminar materials are grown on Van der Waals epitaxy technology, such as the two-dimensional nanostructure of II-VI group semiconductor
Research be also rarely reported.
CdSe and CdS is important II-VI group semiconducting compound, is respectively provided with two kinds of main crystalline substances of buergerite and zincblende
Body structure, potentially valency is applied because their unique physical and chemical properties have in nanoelectronics and opto-electronics
Value, it is prepared and application study has caused the increasing interest of scientists.CdSe band gap is about 1.7eV, its nanometer
Material has extremely excellent fluorescent characteristic, by varying the size of nanoparticle, its fluorescence spectrum can produce from feux rouges to
Change (M.J.Bowers, J.R.McBride, S.J.Rosenthal, White-Light the Emission from of blue light
Magic-Sized Cadmium Selenide Nanocrystals.J.Am.Chem.Soc.2005,127(44),15378–
15379.).And it is with the characteristic such as spectral width is narrow, symmetry is good, fluorescent stability is high, have been widely used for photocatalysis,
The fields such as quantum dot solar cell, light emitting diode.CdS band gap is 2.4eV or so, the higher (104-105cm- of absorption coefficient
1), have the advantages that price is low, preparation process is simple, be widely used as the N-shaped window material of thin-film solar cells, at present people
Most study CdS/CdTe solar cells industrialized production.But the research at present for CdSe and CdS is main
Concentrate in the isostructural preparation of quantum dot, nano wire, nanobelt.And two-dimensional nano of some rarely having based on both materials
The preparation of piece all be use liquid phase method (S.Ithurria, M.D.Tessier, B.Mahler, R.P.S.M.Lobo,
B.Dubertret and Al.L.Efros.Colloidal nanoplatelets with two-dimensional
Electronic structure.Nature Materials.2011,10,936-941.), the nanometer sheet prepared by this method
There are crystallinity is low, size is small, solvent not easy cleaning the shortcomings of, these deficiency constrains it significantly on nano photoelectric device
Using.
Accordingly, it is desirable to provide a kind of height easy to operate, repeated, controllability are strong, and can large area preparation CdSe or CdS bis-
The method for tieing up semiconductor nano material.
The content of the invention
It is an object of the present invention to provide the preparation method of a kind of cadmium selenide or cadmium sulfide two dimension single crystal nanoplate.
In the present invention, applicant employ a kind of new method come large area prepare CdSe and CdS two-dimensional semiconductors receive
Rice material.Different from liquid phase synthesizing method of the prior art, this method is not only easy to operate, it is repeated it is high, controllability is strong, and
The two-dimensional nano piece prepared has the advantages that area is big, dimensional homogeneity is good, crystallinity is high, and it has well with substrate
Compatibility, easy to the making and application of flexible device.Meanwhile material can be transferred to other linings by simple method
Bottom, easy to the research and development and application of extensive photoelectric device.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of preparation method of cadmium selenide or cadmium sulfide two dimension single crystal nanoplate, includes the following steps：
1) material with two-dimensional layered structure is chosen as substrate, using the smooth one side in surface as aufwuchsplate；
2) by CdCl2Powder is put into high-temperature resistant container, is then placed on the heated center region of horizontal pipe furnace, will
Excessive Se powder, which is put into high-temperature resistant container, is placed in heated center upstream apart from heated center 20-26cm, or the S powder by excess
It is put into high-temperature resistant container and is placed in heated center upstream at heated center 24-30cm, substrate is placed in horizontal pipe furnace
Heated center downstream, apart from heated center 5-20cm；
3) to horizontal tube stove evacuation, when pressure is down to 0.1Pa in stove, being filled with inactive gas returns intracavitary air pressure
To atmospheric pressure；
4) 750 DEG C -800 DEG C are warming up to the speed of 20-30 DEG C/min and are kept for 10-15 minutes, during the reaction not
The flow control of active gas is in 15-30sccm；
5) after reaction, treat that tube furnace naturally rings to room temperature, take out substrate, be that growth has cadmium selenide or sulphur on substrate
Cadmium two dimension single crystal nanoplate.
Substantial amounts of experimental verification is carried out by applicant, in technical solution of the present invention, reaction temperature and flow rate of carrier gas are to material
Expect that the influence of growth is maximum.Wherein 750 DEG C -800 DEG C of reaction temperature and the flow rate of carrier gas of 15-30sccm are optimal experiment side
Case.When reaction temperature is excessive, material is easier to be grown to one-dimensional nano line, and the nanometer chip size that when temperature is too low grows it is smaller,
Distribution close packing is unfavorable for the making of large-scale semiconductor device.In addition carrier gas flux it is excessive can also make nanometer sheet growth it is overstocked so as to
Form polycrystalline film.
Preferably, the substrate is mica sheet (Mica), graphene, hexagonal boron nitride or molybdenum sulfide.These types of material is equal
With natural layer structure, it is easy to obtained by the stripping method of " from top to bottom " or the synthetic method of " from bottom to top ".
And its surface it is smooth, without chemical dangling bond, be very beneficial for transferring the sample into the preparation that device is carried out on other substrates, be
The ideal substrate of Van der Waals epitaxial growth.
It is highly preferred that the substrate is mica sheet.Mica sheet is cheap for other stratified materials and is easier to
Obtain, prepared additionally, due to the larger large area for being very suitable for two-dimensional material of its size.Its natural translucency and flexible also profit
In the making of subsequent optical and photoelectricity flexible device.
Preferably, substrate mica sheet is divided into the rectangle of size 2cm*3cm, and mica sheet is dissociated into naturally from centre
Two thin slices, take new dissociation face to be used as growth substrates.Since standing time longer mica sheet is difficult to avoid that ground surface has one
A little cuts or adsorbate, the presence of these impurity influences whether nucleation and the growth of material, therefore selects newly to separate opposite
Clean even curface is as aufwuchsplate.
Preferably, the high-temperature resistant container is ceramic boat, quartz boat, quartz glass tube.
Preferably, the inactive gas is argon gas, nitrogen, helium or neon.
The invention also discloses a kind of cadmium selenide being prepared using preparation method as described above or cadmium sulfide two dimension are single
Brilliant nanometer sheet.
Further, the invention discloses a kind of cadmium selenide as described above or cadmium sulfide two dimension single crystal nanoplate to make
Application in photoelectric device, solar cell, field-effect transistor, visible-light detector and photocatalysis field.
Different from general liquid phase preparation process in the prior art, in the present invention, applicant uses the side of Van der Waals extension
Method prepares large area, CdSe, CdS two-dimensional nano piece of high monocrystalline.The method is characterized in smooth using surface and outstanding without chemistry
The mica sheet of key is substrate, with CdCl2Powder, Se powder or S powder are source material, and inactive gas is carrier gas, under the high temperature conditions
(750 DEG C -800 DEG C of reaction temperatures) CdCl2Steam forms CdSe or CdS steams with Se or S vapor reactions respectively, and then not
(flow rate of carrier gas of 15-30sccm) deposits to forming core on mica sheet under the transporting of active gas, and is epitaxially grown as hexagonal phase
CdSe or CdS two dimension single crystal nanoplates.CdSe the and CdS two-dimensional nano piece arranged regulars that the present invention prepares, crystallinity is high,
There is important researching value and extensive in fields such as solar cell, field-effect transistor, visible-light detector, photocatalysis
Application prospect.
Beneficial effects of the present invention are as follows：
(1) preparation process is simple, and the present invention is reacted using one-step method, only source material need to be put into tube furnace, set load
Throughput and heating program；
(2) production cost is relatively low, CdCl2Powder price is cheap, fusing point is relatively low, can save certain production cost；
(3) repeatability is high, prepares the two-dimensional nano piece success of large area, the CdSe of size uniform and CdS in this way
Rate is high；
(4) controllability is strong, and two-dimensional nano piece is can control by varying conditions such as sedimentation time, evaporating temperature, carrier gas fluxes
Density, thickness, size, shape etc.；
(5) nanometer sheet arranged regular, two-dimensional nano piece and the substrate of the CdSe and CdS of growth have good epitaxial orientation
Relation, has obvious Van der Waals epitaxial growth characteristic；
(6) growth cycle is short, and from reaction is heated to, cooling samples this method to the end, it is only necessary to which four or five hours, take few；
(7) crystallinity is high, and using the chemical vapor deposition under high temperature, the nano material prepared under the conditions of being somebody's turn to do has higher
Crystallinity.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the grower schematic diagram of CdSe and CdS two dimensions single crystal nanoplate of the present invention.
Fig. 2 shows that scanning electron microscope (SEM) picture (a) of CdSe nanometer sheets prepared by the embodiment of the present invention 1 and embodiment 2 are made
The SEM pictures (b) of standby CdS nanometer sheets.
Fig. 3 shows low power atomic force microscope (AFM) picture (a) of CdSe nanometer sheets prepared by the embodiment of the present invention 1, single
The AFM pictures and elevation information (b) of a CdSe nanometer sheets；And the AFM pictures (c) of the CdS nanometer sheets of the preparation of embodiment 2,
The AFM pictures and elevation information (d) of single CdS nanometer sheets.
Fig. 4 shows the CdSe nanometer sheets of the preparation of the embodiment of the present invention 1, the CdS nanometer sheets of the preparation of embodiment 2 at 20 ° to 34 °
X ray diffracting data in the range of the angle of diffraction.
Fig. 5 shows the drawing of CdS nanometer sheets (b) prepared by CdSe nanometer sheets (a), embodiment 2 prepared by the embodiment of the present invention 1
Graceful spectrum.
Fig. 6 shows CdSe nanometer sheets transmission electron microscope (TEM) bright field image (a) of the preparation of the embodiment of the present invention 1, corresponding choosing
Area's electronic diffraction (SAED) picture (b), and high-resolution TEM (HRTEM) image (c)；CdS prepared by the embodiment of the present invention 2 receives
Rice piece TEM bright field images (d), corresponding selective electron diffraction (SAED) picture (e), and HRTEM images (f).
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
(1) preparation of mica sheet substrate：
The 1st, mica sheet is divided into the rectangle of size 2cm*3cm with scissors.
2nd, mica sheet is dissociated into two thin slices naturally from centre with the tapering tweezers in top, new dissociation face is served as a contrast as growth
Bottom.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace.Weigh 0.79 gram
Se powder, is placed in the position of ceramic tube middle-range heated center upstream about 20cm, and mica sheet substrate is put in single temperature zone diamond heating
The downstream at center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 750 DEG C and is kept for 15 minutes, the stream of argon gas during the reaction with the speed of 20 DEG C/min
Speed control is in 15sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out mica sheet substrate, i.e., in mica sheet substrate grown
There are CdSe two dimension single crystal nanoplates.
The grower schematic diagram of CdSe and CdS two dimensions single crystal nanoplate of the present invention is with reference to shown in Fig. 1.Each numeral generation in figure
The implication of table is：1-S powder or Se powder, 2-CdCl2Powder, 3- substrates.
Shown in (a) in scanning electron microscope (SEM) picture such as Fig. 2 of CdSe nanometer sheets manufactured in the present embodiment, most two dimensions
Hexagonal shape is presented in nanometer sheet, and the side of two-dimensional nano piece is all parallel to each other substantially, and it is identical to illustrate that these nanometer sheets have
The orientation of growth, i.e., with obvious Van der Waals epitaxial growth feature.
(a) in Fig. 3 is low power atomic force microscope (AFM) picture of CdSe nanometer sheets, and (b) is single CdSe nanometer sheets
AFM pictures and elevation information.
Fig. 4 shows X ray diffracting data of the CdSe nanometer sheets in the range of 20 ° to the 34 ° angles of diffraction, it was demonstrated that the nanometer sheet
Good crystallinity is respectively provided with, and is hexagonal wurtzite crystal structure.
(a) is the Raman spectrum of CdSe nanometer sheets in Fig. 5, and Characteristic Raman peak LO, 2LO in figure are respectively single order and second order
Longitudinal optical phonon pattern, wherein point and narrow peak also demonstrate that the nanometer sheet of preparation has highly crystalline.
(a) is hexagonal structure CdSe nanometer sheets transmission electron microscope (TEM) bright field image in Fig. 6；(b) it is corresponding Selected area electron
Six sub-symmetry characteristics of rule are presented in diffraction (SAED) picture, diffraction spot, and it is brilliant to correspond to { 10-10 } for the wherein point diffraction of inner ring
Face race, the point diffraction of secondary inner ring correspond to { 11-20 } family of crystal planes, and demonstrating CdSe nanometer sheets again has well monocrystalline
And hexagonal crystallographic texture is presented；(c) it is high-resolution TEM (HRTEM) image of CdSe nanometer sheets, the interplanar distance marked in figure is
0.21nm, it is consistent with the spacing of lattice of CdSe { 11-20 } family of crystal planes.
Embodiment 2
(1) preparation of mica sheet substrate：
The 1st, mica sheet is divided into the rectangle of size 2cm*3cm with scissors.
2nd, mica sheet is dissociated into two thin slices naturally from centre with the tapering tweezers in top, new dissociation face is served as a contrast as growth
Bottom.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace.Weigh 0.32 gram
S powder, is placed in the position of ceramic tube middle-range heated center upstream about 24cm, mica sheet substrate is put in single temperature zone diamond heating
The downstream of the heart, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 750 DEG C and is kept for 15 minutes, the stream of argon gas during the reaction with the speed of 20 DEG C/min
Speed control is in 15sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out mica sheet substrate, i.e., in mica sheet substrate grown
There are CdS two dimension single crystal nanoplates.
Shown in (b) in scanning electron microscope (SEM) picture such as Fig. 2 of CdS nanometer sheets manufactured in the present embodiment, most two wieners
Hexagonal shape is presented in rice piece, and the side of two-dimensional nano piece is all parallel to each other substantially, illustrates that these nanometer sheets have identical life
Long orientation, i.e., with obvious Van der Waals epitaxial growth feature.
(c) in Fig. 3 is low power atomic force microscope (AFM) picture of CdS nanometer sheets, and (d) is single CdSe nanometer sheets
AFM pictures and elevation information.
Fig. 4 shows X ray diffracting data of the CdS nanometer sheets in the range of 20 ° to the 34 ° angles of diffraction, it was demonstrated that the nanometer sheet
Good crystallinity is respectively provided with, and is hexagonal wurtzite crystal structure.
(b) is the Raman spectrum of CdS nanometer sheets in Fig. 5, and Characteristic Raman peak LO, 2LO in figure are respectively single order and second order
Longitudinal optical phonon pattern, wherein point and narrow peak also demonstrate that the nanometer sheet of preparation has highly crystalline.
(d) is hexagonal structure CdS nanometer sheet TEM bright field images in Fig. 6；(e) it is corresponding selective electron diffraction (SAED)
Picture, illustrates that CdS nanometer sheets also have good monocrystalline and presentation hexagonal crystallographic texture；(f) it is the HRTEM of CdS nanometer sheets
Image.
Embodiment 3
(1) preparation of mica sheet substrate：
1. mica sheet is divided into the rectangle of size 2cm*3cm with scissors.
2. mica sheet is served as a contrast from centre is naturally cleaved into two thin slices, new cleavage surface as growth with the tapering tweezers in top
Bottom.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace.Weigh 0.79 gram
Selenium powder, is placed in the position of ceramic tube middle-range heated center upstream about 26cm, and mica sheet substrate is put in single temperature zone tube furnace successively
The downstream of heated center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 800 DEG C and is kept for 10 minutes, the stream of argon gas during the reaction with the speed of 30 DEG C/min
Speed control is in 30sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out mica sheet substrate, i.e., in mica sheet substrate grown
There are CdSe two dimension single crystal nanoplates.The performance parameter of the CdSe nanometer sheets is similar to the product testing result in embodiment 1.
Embodiment 4
(1) preparation of mica sheet substrate：
1. mica sheet is divided into the rectangle of size 2cm*3cm with scissors.
2. mica sheet is served as a contrast from centre is naturally cleaved into two thin slices, new cleavage surface as growth with the tapering tweezers in top
Bottom.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace.Weigh 0.32 gram
Sulphur powder, is placed in the position of ceramic tube middle-range heated center upstream about 30cm, and mica sheet substrate is put in single temperature zone tube furnace successively
The downstream of heated center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high pure nitrogen makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 800 DEG C and is kept for 10 minutes, the stream of nitrogen during the reaction with the speed of 30 DEG C/min
Speed control is in 30sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out mica sheet substrate, i.e., in mica sheet substrate grown
There are CdS two dimension single crystal nanoplates.The performance parameter of the CdS nanometer sheets is similar to the product testing result in embodiment 2.
Embodiment 5
(1) preparation of mica sheet substrate：
1. mica sheet is divided into the rectangle of size 2cm*3cm with scissors.
2. mica sheet is served as a contrast from centre is naturally cleaved into two thin slices, new cleavage surface as growth with the tapering tweezers in top
Bottom.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace, weighs 0.79 gram
Selenium powder, is placed in the position of ceramic tube middle-range heated center upstream about 24cm.Mica sheet substrate is put in single temperature zone tube furnace successively
The downstream of heated center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 780 DEG C and is kept for 12 minutes, the stream of argon gas during the reaction with the speed of 25 DEG C/min
Speed control is in 20sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out mica sheet substrate, i.e., in mica sheet substrate grown
There are CdSe two dimension single crystal nanoplates.The performance parameter of the CdSe nanometer sheets is similar to the product testing result in embodiment 1.
Embodiment 6
(1) preparation of graphene substrate：
1. using the copper foil after acetone and ethanol postincubation as substrate, methane as carbon source, hydrogen as reducing gas,
The chemical vapor deposition experiment of normal pressure is carried out in the atmosphere of argon gas.
2. it is big to obtain high quality by adjusting the conditions such as suitable underlayer temperature, programming rate, growth time on copper foil
The individual layer of area and a small amount of multi-layer graphene.
3. the graphene that copper surface is grown is transferred to silica table by the use of polymethyl methacrylate as protective film
Face.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace, weighs 0.32 gram
Sulphur powder, is placed in ceramic tube middle-range heated center upstream about 28cm positions.Silicon oxide substrate with graphene is put in list successively
The downstream of temperature-area tubular furnace heated center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 780 DEG C and is kept for 12 minutes, the stream of argon gas during the reaction with the speed of 25 DEG C/min
Speed control is in 20sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out graphene substrate, i.e., in graphene-based bottom growth
There are CdS two dimension single crystal nanoplates.The performance parameter of the CdS nanometer sheets is similar to the product testing result in embodiment 2.
Embodiment 7
(1) preparation of hexagonal boron nitride substrate：
1. carried out using the copper foil after acetone and ethanol postincubation as substrate, ammonia borane as carbon source, hydrogen as carrier gas
The chemical vapor deposition experiment of low pressure.
2. the hexagonal boron nitride of large area is obtained by adjusting the conditions such as suitable underlayer temperature, carrier gas flux on copper foil
Atomic layer level thin film.
3. the hexagonal boron nitride that copper surface is grown is transferred to oxidation by the use of polymethyl methacrylate as protective film
Silicon face.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace, weighs 0.79 gram
Selenium powder, is placed in the position of ceramic tube middle-range heated center upstream about 20cm.By the silicon oxide substrate with hexagonal boron nitride successively
It is put in the downstream at single temperature zone diamond heating center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 750 DEG C and is kept for 10 minutes, the stream of argon gas during the reaction with the speed of 20 DEG C/min
Speed control is in 15sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out hexagonal boron nitride substrate, i.e., in hexagonal boron nitride
Substrate grown has CdSe two dimension single crystal nanoplates.The performance parameter of the CdSe nanometer sheets and the product testing result in embodiment 1
It is similar.
Embodiment 8
(1) preparation of molybdenum sulfide substrate：
1. using the oxidized silicon chip after acetone and ethanol postincubation as substrate, molybdenum oxide and sulphur powder as reaction source, argon gas
The chemical vapor deposition experiment of normal pressure is carried out in single temperature zone tube furnace as carrier gas.
2. height is obtained in silicon oxide substrate by adjusting the conditions such as suitable reaction temperature, programming rate, carrier gas flux
The large-sized individual layer of quality and multilayer molybdenum sulfide two-dimensional nano piece.
(2) 0.1 gram of CdCl is weighed2Powder, is then put in the heated center region of tube furnace, weighs 1.0 grams
Selenium powder, is placed in the position of ceramic tube middle-range heated center upstream about 24m.The silicon oxide substrate that grown molybdenum sulfide is put in successively
The downstream at single temperature zone diamond heating center, distance center about 5-20cm.
(3) open mechanical pump to vacuumize, when pressure is down to 0.1Pa in stove, being quickly filled with high-purity argon gas makes intracavitary pressure
Return to atmospheric pressure.
(4) it is rapidly heated to 800 DEG C and is kept for 15 minutes, the stream of argon gas during the reaction with the speed of 20 DEG C/min
Speed control is in 15sccm.
(5) after reaction, treat that tube furnace naturally rings to room temperature, take out molybdenum sulfide substrate, i.e., in molybdenum sulfide substrate grown
There are CdSe two dimension single crystal nanoplates.The performance parameter of the CdSe nanometer sheets is similar to the product testing result in embodiment 1.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (6)
1. the preparation method of a kind of cadmium selenide or cadmium sulfide two dimension single crystal nanoplate, it is characterised in that include the following steps：
1）The material with two-dimensional layered structure is chosen as substrate, using the smooth one side in surface as aufwuchsplate；
2）By CdCl2Powder is put into high-temperature resistant container, is then placed on the heated center region of horizontal pipe furnace, by Se powder
It is put into high-temperature resistant container and is placed in heated center upstream and is put into apart from heated center 20-26cm, or by S powder in high-temperature resistant container
Heated center upstream is placed in apart from heated center 24-30cm, substrate is placed in the heated center downstream of horizontal pipe furnace, distance plus
Thermal center (-tre) 5-20cm；
3）To horizontal tube stove evacuation, when pressure is down to 0.1Pa in stove, being filled with inactive gas makes intracavitary air pressure return to greatly
Air pressure is strong；
4）750 DEG C -800 DEG C are warming up to the speed of 20-30 DEG C/min and is kept for 10-15 minutes, during the reaction torpescence
The flow control of gas is in 15-30sccm；
5）After reaction, treat that tube furnace naturally rings to room temperature, take out substrate, be that growth has cadmium selenide or cadmium sulfide on substrate
Two-dimentional single crystal nanoplate.
2. the preparation method of a kind of cadmium selenide according to claim 1 or cadmium sulfide two dimension single crystal nanoplate, its feature exist
In：The substrate is mica sheet, graphene, hexagonal boron nitride or molybdenum sulfide.
3. the preparation method of a kind of cadmium selenide according to claim 2 or cadmium sulfide two dimension single crystal nanoplate, its feature exist
In：The substrate is mica sheet, and mica sheet is dissociated into two thin slices naturally from centre, takes new dissociation face to be used as aufwuchsplate.
4. the preparation method of a kind of cadmium selenide according to claim 1 or cadmium sulfide two dimension single crystal nanoplate, its feature exist
In：The high-temperature resistant container is ceramic boat, quartz boat or quartz glass tube.
5. the preparation method of a kind of cadmium selenide according to claim 1 or cadmium sulfide two dimension single crystal nanoplate, its feature exist
In：The addition of the Se powder or S powder according to CdCl2The stoichiometric ratio reacted is excessive.
6. the preparation method of a kind of cadmium selenide according to claim 1 or cadmium sulfide two dimension single crystal nanoplate, its feature exist
In：The inactive gas is argon gas, nitrogen, helium or neon.
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